42results about How to "Guaranteed optical purity" patented technology

The present invention relates to a method for preparing a novel S-(-)-amlodipine, and especially to a novel method for preparing S-(-)-amlodipine through the resolution of racemic amlodipine. The N,N-dimethylformamide (DMF) is used as a dissolvent. The L-(+)-tartaric acid is used as a resolving agent. Not only can the excellent resolving effect be obtained, but also the cost is low and safety is excellent.

The invention provides a new enantioselective process for the preparation of (S) -pregabalin, or a pharmaceutical acceptable addition acid salt comprising: acid hydrolysis of the dioxolan ring of a chiral compound of general formula (I) to obtain compound of general formula (II); oxidation of compound (II) to obtain a compound of general formula (III) and transforming compound (III) into compound of general formula (IV); subjecting compound (IV) to basic hydrolysis to obtain a compound of general formula (V) which is reduced to obtain enantiomerically pure S-pregabalin. The invention also provides new chiral intermediates involved in the process.

The invention discloses a preparing method for di-fatty acid glycerol phosphatidyl glyceride. The preparing method includes the steps that (S)-1,2-fatty glyceride serves as a raw material, and is reacted with 2-cyano ethyl diisopropyl chloro -amidophosphoric acid or di-(diisopropyl amino) (2-cyano ethyoxyl) phosphine and 2,2-dimethyl-4-hydroxymethyl-1,3-dioxolame in sequence, then phosphate ester is generated under the condition of iodine oxidation, finally all protecting groups are removed under the ammonia water condition and the weak acid condition, and the (R)-1,2-di-fatty acid glycerol phosphatidyl glyceride is obtained. According to the method, the raw materials are low in cost and easy to obtain, the reaction conditions are mild, the steps are simple, and the method is suitable for industrial production.

The invention discloses a preparation method of tamsulosin hydrochloride with high optical purity, and belongs to a medicine technology and a chemical field. A recrystallization method is adopted, crude products of (R)-5-(2-(2-(2-ethoxyphenoxy) ethyl amino) propyl)-2-methoxyl phenyl sulfonamide hydrochloride are refined, so that pure products of the (R)-5-(2-(2-(2-ethoxyphenoxy) ethyl amino) propyl)-2-methoxyl group sulfonamide hydrochloride of which the e.e. value is larger than 99.8% is obtained; a crystallizing solvent adopted by the recrystallization method is a mixed solvent consisting of an organic solvent and water, the organic solvent is selected from one of methanol, ethyl alcohol, acetone, acetonitrile and isopropyl alcohol, and the recrystallization temperature is under 15 DEG C. The preparation method disclosed by the invention is simple to operate, short in period, low in cost and good in repeatability, and can solve the inevitable problem of rework for treatment in the industrial production.

The application provides a compound of formula I and a preparation method thereof. The application also provides the use of the compound of formula I for synthesizing buvaracetam and the synthesis method. The raw materials involved in the method described in this application are easy to obtain and cheap, and can prepare brivaracetam with high optical purity.

The invention discloses a method for preparing D-sulbenicillin sodium. The method includes steps of removing L-amino acid from L-amino acid salt of D-sulfophenylacetic acid in solvents and carrying out salt forming to obtain D-sulfophenylacetic acid salt; carrying out reaction on the D-sulfophenylacetic acid salt and acylating agents to obtain mixed acid anhydride; dissolving 6-APA in organic solvents under the effect of organic alkali; dropwise adding mixed acid anhydride solution into 6-APA solution, and carrying out sufficient reaction and after-treatment to obtain the D-sulbenicillin sodium. The D-sulfophenylacetic acid is an intermediate. The 6-APA is a matrix. The method has the advantages that the D-sulbenicillin sodium is prepared by the aid of novel synthetic routes, conditions are mild, the method includes stable process and is easy to implement, and the problems of instable processes of existing methods or insufficient optical purity of products and the like can be solved bythe aid of the method.

Disclosed is a method that is for producing 1-bromo-1-[3,5-bis(trifluoromethyl)phenyl] ethane having high optical purity, and that is a method containing a step for brominating optically active 1-[3,5-bis(trifluoromethyl)phenyl] ethanol using, as a brominating agent, either a) the combination of a phosphorus halide and hydrogen bromide, b) the combination of 1,2-dibromo-1,1,2,2-tetrachloroethane and the organophosphorus compound represented by general formula I, which is P(R1)(R2)(R3) (in the formula: R1, R2 and R3 each independently indicate a C6-10 aryl group, a C6-10 aryloxy group, a C1-10 alkyl group, a C1-10 alkoxyl group, a C3-6 cycloalkyl group, or a C3-6 cycloalkoxyl group), or c) the combination of N-bromosuccinimide and a dialkyl sulphide.

The invention provides a preparing method for tiagabine hydrochloride, which includes the following operating steps: firstly, taking tiagabine ethyl ester to be dissolved in solvent, adding L-configuration organic acid, performing heating reflux until the tiagabine ethyl ester is completely dissolved, then performing reflux for 30-60 min, cooling to the room temperature, cooling and crystallizing at the temperature of minus 30 -minus 20 DEG C, and collecting a solid matter A; secondly, adding solvent in the solid matter A, performing heating reflux until the tiagabine ethyl ester is completely dissolved, then performing reflux for 30-60 min, cooling to the room temperature, cooling and crystallizing at the temperature of minus 10-0 DEG C, and collecting a solid matter B; thirdly, dissolving the solid matter B, sequentially adding sodium hydroxide and hydrochloric acid to react, extracting and recrystallizing, so as to obtain the tiagabine hydrochloride. The preparing method provided by the invention not only remarkably improves the productivity by 90% above, but also guarantees the 99.9% of chemical and optical purity, is simple and convenient to operate, has no special requirement for equipment, and is more suitable for large-scale industrial production.

The invention relates to the field of chemistry, particularly a preparation method of a key intermediate (S)-3-hydroxypyrrolidine hydrochloride of darifenacin for treating overactive bladder syndrome and an antihypertensive drug barnidipine. The preparation method comprises the following steps: carrying out Mitsunobu reaction on (R)-1-N-tert-butyloxycarbonyl-3-hydroxypyrrolidine so as to be condensed with acid to obtain an upturned-structure ester, hydrolyzing ester bond under alkaline conditions to obtain (S)-1-N-tert-butyloxycarbonyl-3-hydroxypyrrolidine, and removing Boc protecting groups under acidic conditions, thereby finally obtaining the key intermediate. The method is simple and easy to implement, has the advantages of cheap and accessible raw materials, lower cost and high yield, and has potential production value.

The invention discloses a preparation method of (S)-N-glycidol phthalimide in a structural formula 1. The method comprises the following steps of: I, phthalimide salt of a structural formula 9 and a compound of a structural formula 10 are subjected to heating reflux for reaction in an alcohols solvent to obtain the compound of a structural formula 11; II, the compound of the structural formula 11 obtained form the step I is reacted with the compound of a structural formula 12 in an aprotic solvent under the action of alkaline to obtain a (S)-N-glycidol phthalimide crude product of the structural formula 1; and III, the (S)-N-glycidol phthalimide crude product of the structural formula 1 obtained from the step II is refined by ethanol to obtain the (S)-N-glycidol phthalimide with the optical purity larger than or equal to 99.0%. The preparation method is simple to operate and good in safety, the optical purity of the obtained product is high (larger than or equal to 99.0%), and the preparation method is suitable for industrial production. The invention also discloses a novel synthetic method of Rivaroxaban.

The invention discloses a method for simultaneously detecting a key intermediate (formula 2) and a corresponding isomer (formula 3) of afatinib. According to the method, isocratic elution is performed on a high performance liquid chromatograph; a chromatographic column which takes cellulose-tris(3,5-dimethyl phenylcarbamate) as a filling agent is adopted; a flow phase is a mixed solution of n-hexane, isopropyl alcohol and acetonitrile. Through the method, the key intermediate (formula 2) and the corresponding isomer (formula 3) of the afatinib can be effectively separated and detected, and the separation degree can reach 2.0 or higher.

The invention discloses a preparation method of tamsulosin hydrochloride with high optical purity, and belongs to a medicine technology and a chemical field. A recrystallization method is adopted, crude products of (R)-5-(2-(2-(2-ethoxyphenoxy) ethyl amino) propyl)-2-methoxyl phenyl sulfonamide hydrochloride are refined, so that pure products of the (R)-5-(2-(2-(2-ethoxyphenoxy) ethyl amino) propyl)-2-methoxyl group sulfonamide hydrochloride of which the e.e. value is larger than 99.8% is obtained; a crystallizing solvent adopted by the recrystallization method is a mixed solvent consisting of an organic solvent and water, the organic solvent is selected from one of methanol, ethyl alcohol, acetone, acetonitrile and isopropyl alcohol, and the recrystallization temperature is under 15 DEG C. The preparation method disclosed by the invention is simple to operate, short in period, low in cost and good in repeatability, and can solve the inevitable problem of rework for treatment in the industrial production.

The present invention discloses one kind of 3-hydroxy olefine acid derivative in the structure as shown and its preparation process and application. By means of the inherent chirality of the material and the cross-metathesis of olefine, the product of the present invention, 3-hydroxy olefine acid, has high optical purity. The present invention lays foundation for the industrial preparation of 3-hydroxy olefine acid derivative.

The invention provides a method for preparing valsartan. The method comprises the following steps: firstly, reacting N-(triphenylmethyl)-5-(4'-formyl-biphenyl-2-yl) tetrazolium with sodium methoxide, secondly, adding dichlorodicyanobenzoquinone (DDQ) and oxidizing, thirdly, reacting with L-valine methyl ester, fourthly, alkylating with valeryl chloride, fifthly, removing triphenylmethyl group and sixthly removing ester group and acidifying to obtain the target product valsartan. According to the method, a novel method for preparing valsartan is provided by virtue of the Williamson ether synthesis step and DDQ oxidation step, since potassium dihydrogen phosphate is adopted as a buffering reagent in the triphenylmethyl group removal process and a 1.3mol / L sodium hydroxide solution is used in the hydrolysis process, the problem of racemization of the product generated caused by too strong alkaline is avoided and the method is of important significance in maintaining the optical purity of the valsartan product.

The invention relates to a high-activity double-function catalyst as well as a preparation method and application of the high-activity double-function catalyst. The catalyst is a tetradentate schiff base aluminum complex and the molecule contains more than one quaternary ammonium salt or quaternary phosphonium salt radical. Under a low catalyst concentration, the high-activity double-function catalyst still has the higher catalytic activity; reaction conditions are relatively moderate and a process is simple and convenient; the catalytic efficiency is high and the product selectivity is high; any organic solvent does not need to be added; and when chiral epoxyalkane is used as a reactant, the optical purity of a product can be completely kept.

The invention discloses a method for preparing L-theanine by a chemical method. The method comprises the following steps: firstly, reacting ethylamine with acryloyl chloride in the presence of an alkali to obtain N-ethylacrylamide; secondly, perform Michael addition reaction on chiral auxiliary BPB based glycine Schiff base Ni(II) coordination compound and the N-ethylacrylamide in the presence ofthe alkali to obtain theanine Schiff base Ni(II) coordination compound; and finally, performing acid hydrolysis on the theanine Schiff base Ni(II) coordination compound to prepare the L-theanine. Themethod adopts the chiral auxiliary chemical method to prepare the L-theanine, and constructs a complete theanine fragment through the Michael addition reaction so as to prepare the theanine Schiff base Ni(II) coordination compound, wherein the rigid space structure of the coordination compound can maintain the L-configuration of the theanine so as to ensure the optical purity of the L-theanine. The method can reclaim the chiral auxiliary in high yield, and can elute Ni(II) ions through ion exchange for recycling.

The invention discloses a method for preparing D-sulbenicillin sodium. The method includes steps of removing L-amino acid from L-amino acid salt of D-sulfophenylacetic acid in solvents and carrying out salt forming to obtain D-sulfophenylacetic acid salt; carrying out reaction on the D-sulfophenylacetic acid salt and acylating agents to obtain mixed acid anhydride; dissolving 6-APA in organic solvents under the effect of organic alkali; dropwise adding mixed acid anhydride solution into 6-APA solution, and carrying out sufficient reaction and after-treatment to obtain the D-sulbenicillin sodium. The D-sulfophenylacetic acid is an intermediate. The 6-APA is a matrix. The method has the advantages that the D-sulbenicillin sodium is prepared by the aid of novel synthetic routes, conditions are mild, the method includes stable process and is easy to implement, and the problems of instable processes of existing methods or insufficient optical purity of products and the like can be solved bythe aid of the method.