45results about How to "Moderate yield" patented technology

The invention relates to synthesis of organic compounds, and provides a method for preparing potassium trifluoroborate series compounds. The method comprises the following steps of: adding organic boric acid or organic borate and solvent (THF (tetrahydrofuran), or MTBE (Methyl Tertiary Butyl Ether), or ethyl acetate, or methanol) into a reaction kettle lined with tetrafluoroethylene plastic at room temperature; adding potassium bifluoride and water at normal temperature, stirring for 1 to 12 hours, and reacting to prepare a solid-liquid mixture; adding solid potassium ion containing inorganic or organic alkali into the solid-liquid mixture after the reaction is completed, neutralizing until the pH is between 7 and 9, and continuously stirring for 1 to 5 hours; directly filtering to obtain a solid coarse product after stirring is completed; dissolving the coarse product with solvent, filtering and concentrating, adding nonpolar solvent, and pulping to obtain high-quality RBF3K series compounds. The method is easy to operate, has mild reaction conditions, and can realize scale-up production; and the product prepared by the method has high yield and excellent purity, and the cost is greatly reduced.

The invention relates to a synthesis method of tert-butyl-1, 7-diazaspiro [3.5] nonane-1-formate, and mainly solves the technical problem that no suitable industrial synthesis method exists at present. The method comprises the following seven steps: 1, reacting a compound 1 with ethyl malonate added into a solvent ethanol to obtain a compound 2; 2, reacting the compound 2 with lithium borohydridein tetrahydrofuran to obtain a compound 3; 3, reacting the compound 3 with p-toluenesulfonyl chloride in dichloromethane to obtain a compound 4; 4, adding cesium carbonate into the compound 4 in acetonitrile serving as a solvent for cyclization to obtain a compound 5; 5, adding magnesium chips into the compound 5 in methanol serving as a solvent for reduction to obtain a compound 6, 6, reacting the compound 6 with Boc anhydride in dichloromethane to obtain a compound 7, and 7, reacting the compound 7 with palladium on carbon in methanol to obtain a final compound 8.

The invention discloses a preparation method of palbociclib for treating breast cancer. The method comprises the following steps: 1) enabling N-cyclopentyl-2-methoxyl-3-cyan-4-methyl-5-acetyl-6-oxopiperidine-2-alkene and N-[5-(1-piperazinyl)-2-pyridyl] guanidine in the presence of N, N-Mes imidazolium salt to carry out a contact reaction to obtain 6-acetyl-8-cyclopentyl5-methyl-2-[[5-(1-piperazinyl)-2-pyridyl]amino]-5,6-dihydropyridino-[2,3-d]pyrimidine-7(8H)-ketone, wherein the temperature of the contact reaction is 85-100 DEG C; and (2) enabling 6-acetyl-8-cyclopentyl5-methyl-2-[[5-(1-piperazinyl)-2-pyridyl]amino]-5,6-dihydropyridino-[2,3-d]pyrimidine-7(8H)-ketone obtained in step 1) to carry out a dehydrogenation reaction in the presence of a dehydrogenation accelerant to generate palbociclib. The method is simple, is mild in condition and is capable of improving the yield and shortening the reaction time.

The invention discloses a synthesis method of N-(1-ethyl propyl)-3, 4-dimethylaniline, and the method comprises reaction of 3, 4-dimethyl nitrobenzene, pure hydrogen and 3-pentanone under the joint action of various catalysts at the reaction temperature of 40-55 DEG C and under the pressure reaction of 0.1MP-0.5MP hydrogen. The various catalysts comprise (a) a platinum carbon catalyst; and a (b) phosphoric acid-sodium dihydrogen phosphate acid buffer solution. The one step synthesis method of the N-(1-ethyl propyl)-3, 4-dimethylaniline is low in reaction temperature, short in reaction time and simple in process, the raw material 3, 4-dimethyl nitrobenzene can be completely transformed, and the yield of the product N-(1-ethyl propyl)-3, 4-dimethylaniline under optimized conditions is 99.8%.

Novel processes for preparing arylsulfur pentafluorides are disclosed. Processes include reacting at least one aryl sulfur compound with a halogen and a fluoro salt to form an arylsulfur halotetrafluoride. The arylsulfur halotetrafluoride is reacted with a fluoride source to form a target arylsulfur pentafluoride.

The invention relates to 1,1-diacetate synthesis catalyzed by sulfonated cage-type mesoporous carbon. The method is characterized in that aldehyde and acetic anhydride are placed in a reactor according to a molar ratio of 1:1-3; a sulfonated cage-type mesoporous carbon catalyst is added, wherein 5-20mg of the sulfonated cage-type mesoporous carbon catalyst is added to each mole of aldehyde; the materials are stirred under room temperature until a reaction is sufficiently carried out; ethyl acetate with a volume 20-30 times that of the reaction liquid is added; the catalyst is removed by filtering; a filtrate is washed three times by using a saturated NaHCO3 water solution, and once by using water; an organic phase is dried by using anhydrous Na2SO4; the solvent is removed by reduced-pressure distillation under a pressure of 0.09MPa, such that a crude product is obtained; and re-crystallization or column chromatographic separation is carried out, such that 1,1-diacetate is obtained. Compared with existing 1,1-diacetate synthesizing method, the method provided by the invention has the advantages of short reaction time, high yield, mild reaction condition, recyclable catalyst, and the like. The method can be used for synthesizing 1,1-diacetate.

The invention relates to a brewing process of sweet sparkling apple wine. The process comprises the following steps: (1) soft-pressing juice taking by an extrusion method; (2) juice clarification; (3)low-temperature concentration and separation; (4) temperature-controlled fermentation; (5) pressure-maintaining low-temperature fermentation; (6) sugar-maintaining termination fermentation; and (7) clarification filtering treatment. The physicochemical indexes are as follows: the alcoholic strength is 11.5-12.0 (v / v)%, the reducing sugar content is greater than or equal to 95.0 g / L, the total acidity is 8.0-9.0 g / L, the free SO2 content is less than or equal to 50mg / L, the total SO2 content is less than or equal to 150mg / L, the volatile acid content is less than or equal to 0.8 g / L, and the pressure is 0.25-0.35 MPa. The process has the advantages that the juice is extracted through soft pressing, so that the influence of bitter substances on the aroma, taste and quality of the juice is reduced; the aroma and sugar of the fruit juice are concentrated through a low-temperature concentration technology; and through low-temperature pressure-maintaining fermentation and sugar-maintainingtermination fermentation, the finished wine is beautiful and light golden yellow. The finished wine is clear and transparent, bubbles are lasting and fine, and the finished wine has typical apple aroma and nectar aroma, strong fruity aroma, elegant and pure wine aroma, mellow and mellow taste, fullness, coordination, complexity, balance, and fragrant, fresh and lasting aftertaste.

The invention relates to a brewing process of mixed fragrance type sparkling sweet apple wine. The brewing process comprises the following steps: step 1, carrying out soft-pressing to take juice; steptwo, adjusting the acidity of lemon juice; step three, carrying out clarification of fruit juice; step four, carrying out concentration and separation at a low temperature; step five, carrying out temperature-controlled fermentation; step six, carrying out clarification and filtering; step seven, carrying out pressure-maintaining secondary fermentation; step eight, carrying out incomplete fermentation termination; step nine, carrying out low-temperature ageing; and step ten, carrying out clarification and filtration treatment under the conditions of setting physical and chemical indexes as follows: 11.5 to 12.0 (v / v) percent of the alcoholic strength, reducing sugar being greater than or equal to 95.0 g / L, total acidity of 8.0 to 9.0 g / L, free SO2 being less than or equal to 50mg / L, totalSO2 being less than or equal to 150mg / L, volatile acid being less than or equal to 0.8g / L, and the pressure of0.25 to 0.35 MPa. The brewing process has the following advantages: after the process operation, the influence of easy oxidation and browning of the apples after juicing on the aroma, taste and quality of the juice is reduced; the acidity of the apple juice is adjusted by lemon juice, sothat the complexity of the fragrance and the taste of the apple juice are increased; the oxidation resistance of the apple juice is improved; with the low-temperature concentration technology, the pressure-maintaining secondary fermentation technology, the incomplete fermentation termination technology and the low-temperature ageing technology with yeast paste, the yeast fragrance is enhanced while the wine fragrance contains the fine apple fragrance and elegant lemon fragrance, so that the aroma richness is improved, the taste is more mellow and complex, and the sweetness is pure and clean without sweet greasy feeling.

The invention relates to a preparation method of entecavir. The method comprises the steps: by adopting butanedial as a raw material, firstly synthesizing optically pure double-loop olefine aldehyde in the presence of a catalytic amount (R)-proline and dibenzylamine trifluoroacetate, protecting hydroxyl by using methyl, and carrying out decarbonylation by utilizing chlorotris(triphenylphosphine)-rhodium as a catalyst to obtain (3aS, 6aR)-2-methoxyl-3,3a-6,6a-tetrahydro-2H-cyclopentano [b] furan; carrying out Prins reaction in the presence of sulfuric acid to obtain a reduzate of Corey lactone, carrying out deprotection on all hydroxyls by using TBS, selectively removing a 2-bit protecting group and carrying out decarboxylic reaction in the presence of lead acetate to obtain a methylene compound; and finally introducing guanine by adopting a conventional method and carrying out deprotection to obtain the entecavir. By adopting butanedial as an initial raw material, the method has less than ten steps, and is mild in reaction condition, available in raw material and reagent, simple in operation, moderate in yield and suitable for industrial production.

The invention relates to novel cell-penetrating fluorescent dyes with secondary alcohol functionalities having one of the following general formulae I-III and 4: The invention also relates to the use of these compounds for optical microscopy and imaging techniques.

The invention relates to camptothecin, in particular relates to homocamptothecin compounds and a synthesis method thereof, and mainly solves the technical problems of poor solubility and bioavailability of homocamptothecin in the prior art. Structural formulas of the homocamptothecin compounds are as shown in I and II, and the homocamptothecin compounds comprise racemic compounds and (S)-and (R)-stereisomers corresponding to the racemic compounds. The invention specifically relates to derivation of 10-hydroxyl homocamptothecin compound, the 10-hydroxyl homocamptothecin is used as a mother nucleus for synthesis of a series of homocamptothecin ester and amide compounds. The invention provides a new synthetic route, and according to the path, a full synthesis ring enlargement method is not needed, and protection and deprotection are not needed.

The invention discloses a synthesis method of a polysubstituted benzo[c, d] indole compound. The synthesis method comprises the following steps: taking an 8-alkynyl naphthylamine compound, a catalystand alkali according to a molar ratio of 1:(0.1-0.5):(1-2), and putting into a reaction container; adding a solvent into the reaction container until the 8-alkynyl naphthylamine compound is totally dissolved; putting the reaction container in an oil bath at 0-100 DEG C, and stirring for reacting for 0-24h; cooling to room temperature; filtering with kieselguhr or silica gel powder; flushing the filter residue with dichloromethane for 2-4 times; combining the filtrates and performing reduced-pressure distillation to remove the solvent; separating with a silica gel chromatographic column, and performing reduced-pressure distillation to obtain the polysubstituted benzo[c, d] indole compound. According to the synthesis method disclosed by the invention, the polysubstituted benzo[c, d] indole compound is synthesized by a one-pot one-step process, the processes of intermediate separation and purification are reduced, and the operation method is simple; moreover, the reaction conditions are mild, the reaction selectivity is high, the yield is high, the substrate is widely applicable, the reaction raw materials are simple and easily available, and the production cost is low; the synthesismethod is suitable for small-scale preparation in a laboratory as well as industrial large-scale production.

The invention discloses a novel ceramide analogue B, and a preparation method and application thereof, and belongs to the technical field of medicines. On one hand, the invention further provides thenovel ceramide analogue B, and on the other hand, the invention provides the preparation method and application of the novel ceramide analogue B. The synthetic condition of the novel ceramide analogueB disclosed by the invention is mild and is easy to control, the yield is moderate, and industrialization is easy. The novel ceramide analogue B provided by the method is more easily combined with enzymes, can inhibit proliferation of tumor cells, and also has obviously influence on differentiation and period of leukemia tumor cells, and multi-way tumor resistance can be facilitated.

The invention relates to a truxeneone-benzophenanthrene disk-shaped liquid crystal organic semiconductor material and a preparation method thereof. The method includes adding monobromobenzophenanthrene and potassium carbonate into N, N'-dimethylformamide, adding a trihydroxytruxene compound under the protection of inert gases, heating to the temperature of 80 DEG C to conduct a reaction for 36-48hours while stirring, removing the gas protection, and exposing the reaction system in the air to continue heating for 24-36 hours of reaction; after the reaction is completed, cooling reaction liquidto room temperature, pouring the reaction liquid into ice water to precipitate out red solids, performing suction filtration to obtain a crude product, performing vacuum drying, purifying the crude product through column chromatography isolation, taking dichloromethane as eluent, and recrystallizing a mixed organic solvent, and performing vacuum drying. The synthesis method has the advantages ofsimple operation, mild reaction condition and moderate yield, and the reactions of etherification-based polymer construction and oxidation-based truxeneone acquisition are connected in series by one step, and the p-n type disk-shaped liquid crystal compound is successively synthesized; the efficient preparation method is provided for complex truxeneone derivatives.

The invention relates to 1,1-diacetate synthesis catalyzed by sulfonated cage-type mesoporous carbon. The method is characterized in that aldehyde and acetic anhydride are placed in a reactor according to a molar ratio of 1:1-3; a sulfonated cage-type mesoporous carbon catalyst is added, wherein 5-20mg of the sulfonated cage-type mesoporous carbon catalyst is added to each mole of aldehyde; the materials are stirred under room temperature until a reaction is sufficiently carried out; ethyl acetate with a volume 20-30 times that of the reaction liquid is added; the catalyst is removed by filtering; a filtrate is washed three times by using a saturated NaHCO3 water solution, and once by using water; an organic phase is dried by using anhydrous Na2SO4; the solvent is removed by reduced-pressure distillation under a pressure of 0.09MPa, such that a crude product is obtained; and re-crystallization or column chromatographic separation is carried out, such that 1,1-diacetate is obtained. Compared with existing 1,1-diacetate synthesizing method, the method provided by the invention has the advantages of short reaction time, high yield, mild reaction condition, recyclable catalyst, and the like. The method can be used for synthesizing 1,1-diacetate.

The invention discloses an improved method for preparing penfuridol, comprising the following steps: using 4, 4-bis (4-fluorophenyl) butyric acid as a starting material, carrying out reduction synthesis to synthesize an intermediate I [4, 4-bis (4-fluorophenyl)-1-butanol]; carrying out esterification with a sulfonyl chloride compound to synthesize an intermediate II [4, 4-bis (4-fluorophenyl)-1 (4-methyl-phenyl)-butyl sulfonate] or [4, 4-bis (4-fluorophenyl)-1-methyl-butyl sulfonate]; and condensing with pipradrol to obtain penfuridol. According to the preparation method, 4, 4-bis (4-fluorophenyl) butyric acid is used as a raw material, penfuridol is obtained through a reduction reaction, an esterification reaction and a condensation reaction, the total yield is 81.3%, the whole process isconvenient to operate and mild in reaction, the obtained product is high in yield and purity, and the preparation method is more economical and more suitable for industrial application. The technicalproblems that an existing method is low in yield and poor in purity are solved. The reaction general formula is as shown in the specification.

The invention discloses a synthesis method of 1H-pyrrolo[2,3-b]pyridine-2-boronic acid pinacol ester, and belongs to the field of medicinal chemistry. The synthesis method comprises the following steps: reacting 7-azaindole serving as a raw material with di-tert-butyl dicarbonate to synthesize 1H-pyrrolo[2,3b]pyridine-1-carboxylic acid tert-butyl ester, reacting the 1H-pyrrolo[2,3b]pyridine-1-carboxylic acid tert-butyl ester with n-butyl lithium and 1,2-dibromotetrafluoroethane at low temperature to synthesize 2-bromo-1H-pyrrolo[2,3-b]pyridine, synthesizing 2-bromo-1H-pyrrolo[2,3-b]pyridine-1-carboxylic acid tert-butyl ester, removing the protective group to obtain 2-bromo-1H-pyrrolo[2,3-b]pyridine, and reacting 2-bromo-1H-pyrrolo[2,3-b]pyridine with bi-pinacol borate under the catalytic action of transition metals to obtain the target product. The raw materials and reagents are cheap and easy to obtain, reaction conditions are mild, the safety is high, the cost is low, and the preparation method is easily applied to industrial batch production.

The present application relates to novel methods for the preparation of secondary carbinamine compounds, particularly the preparation of secondary carbinamine compounds of the formula Ia, formula Ib or formula IV from aldehydes of the formula II and boronic acids of the formula III or formula V, in the presence of ammonia or an ammonia equivalent of the formula NH4+X−.