53 results about "Trimethylsilyl iodide" patented technology

The invention relates to a preparation process of trimethyliodosilane, which has the advantages of moderate reaction conditions, simple process, safety in operation, high yield and extremely few three wastes. The preparation process takes anhydrous sodium iodide, anhydrous lithium chloride and trimethylchlorosilane as raw materials and the raw materials react in a dried nitrogen atmosphere to synthesize the trimethyliodosilane. According to the method provided by the invention, a traditional complicated process of preparing trimethyliodosilane from hexamethyldisilane and hexamethyldisiloxane is changed; reaction conditions are moderate and operation is safe; dangers of utilizing high-danger chemicals including metal potassium and sodium are avoided; meanwhile, a high-temperature iodization difficulty is also avoided; in a whole production circulating process, only the trimethyliodosilane product and a byproduct sodium chloride are produced and other three wastes are not generated, so that the process is green and environmental-friendly.

The invention discloses a steroid environment endocrine disturbing chemicals hydroxyl group / keto group synchronous derivatization method of steroid environment endocrine disturbing chemicals (oestrone, 17 beta-estradiol, 17 alpha-ethinyl estradiol, estriol and progesterone). The method comprises the following steps: first fetching standard mixed solution containing the steroid environment endocrine disturbing chemicals and internal standard and introducing high-purity nitrogen at normal temperature so as to dry the standard mixed solution; and adding derivatization reagent prepared from N-methyl-N-trimethylsilyl trifluoroacetamide, iodotrimethylsilane and dithiothreitol based on a proportion of 1,000 muL:5 to 10 muL:5 mg and reacting at 20 to 60 DEG C for 5 to 10 min so as to obtain the derivatization product shown in figure. The method has the advantages of simple and time-saving operation, low energy consumption and cost and the like. The hydroxyl group and the keto group can be derivatized synchronously, the linear correlation among the derivatization products is good, and the detection limit of instrument can reach 0.01 to 1 pg / mu L. The method can be used for the GC-MS detection of the steroid environment endocrine disturbing chemicals in samples such as water, bottom sediment, organisms and the like.

The invention relates to a method for synthesizing cefquinome sulfate and relates to a preparation method of a medicament for animals. The preparation method comprises the following steps: taking cefotaxime, 2,3-cyclohexyl pyridine and trimethyliodosilane as initial raw materials; preparing cefotaxime hydriodate from the cefotaxime; carrying out decoloring and silica column chromatography on the cefotaxime; and reacting the treated cefotaxime with sulphuric acid to prepare a cefquinome sulfate product. Compared with the prior art, the invention has the advantages of high yield of products, stable production quality and suitability for industrial production.

The invention discloses a method for preparing cefepime hydrochloride. The method comprises the following steps of: adding hexamethyldisilazane and trimethylsilyl iodide into 7-aminocephalosporanic acid (ACA), performing vacuum reflux at the temperature of 55 DEG C for 12h, reducing the temperature, diluting, adding N-methylpyrrolidone and trimethylsilyl iodide, reacting at the temperature of 40 DEG C for 23h, after-treating and recrystallizing to obtain 7-ACMP.HCl, dissolving the 7-ACMP.HCl into a solvent at the temperature of 0 to 5 DEG C, adding a small amount of AE-active ester and triethylamine for multiple times, and treating to obtain the cefepime hydrochloride after the reaction is finished. The method for preparing the cefepime hydrochloride is high in reaction speed, low in production cost, and high in product purity and flowability.

The invention relates to a method for synthesizing cefquinome sulfate and relates to a preparation method of a medicament for animals. The preparation method comprises the following steps: taking cefotaxime, 2,3-cyclohexyl pyridine and trimethyliodosilane as initial raw materials; preparing cefotaxime hydriodate from the cefotaxime; carrying out decoloring and silica column chromatography on the cefotaxime; and reacting the treated cefotaxime with sulphuric acid to prepare a cefquinome sulfate product. Compared with the prior art, the invention has the advantages of high yield of products, stable production quality and suitability for industrial production.

The present invention discloses a synthetic method of lamivudine intermediate, the method comprises the following steps: a compound of formula V is obtained by methoxylation reaction of a compound of formula VI and a hydrochloric acid methanol solution; a compound of formula IV is obtained by reduction reaction of the compound of formula V and sodium borohydride in ethanol; a compound of formula III is obtained by esterification reaction of the compound of formula IV and chlorinated carbonate under the effect of an organic base for formation of bicyclic carboxylic ester; a compound of formula II is obtained by acylation reaction of the compound of formula III and acetic anhydride under the acid catalysis; a meso compound of the formula I' is obtained by glycosylation reaction of the compound of formula II and silane protected N4-acetamido cytosine under the Iodotrimethylsilane catalysis; and the lamivudine intermediate as shown in the formula I is obtained by recrystallization resolution of the meso compound of the formula I'. The method has the advantages of being simple in operation, low in cost, high in product purity, and the like.

The invention discloses a preparation method of cefpirome hydriodate. According to the method, under a condition of the presence of excess trimethyliodosilane in a reaction system, dilute hydrochloric acid is used for replacing a mixed liquid of potassium iodide and hydrochloric acid in the prior art for crystallization, thus cefpirome hydriodate residues are reduced to zero, and at the same time, the product yield is ensured.

The invention relates to a synthesis method for making cefpirome sulfate. The method comprises the following steps that: cefotaxime and 2, 3-cyclopenopyridine, with the molar ratio of between 1:7 and 1:12, are mixed with trimethyl bromosilicane used as protecting agent inside organic solvent to carry out substitution reaction, thereby generating cefpirome dihydrobromide; and the salt-forming reaction of the cefpirome dihydrobromide is carried out to make cefpirome sulfate. According to the synthesis method of cefpirome sulfate provided by the technical proposal of the invention, cefotaxime and trimethyl bromosilicane are respectively used as raw material and protecting agent to make cefpirome sulfate. Because enough supply and technical maturity of cefotaxime are realized in China and trimethyl bromosilicane is more active than trimethylchlorosilane and is cheaper than trimethyliodosiliane, the synthesis method has the advantages of low cost of raw material, high yield, simple synthetic route and convenient operation.

The invention relates to a preparation method of cefalonium. According to the preparation method, raw materials (cefalotin and pyrazinamide) react at a low temperature to obtain the product cefalonium. The preparation method particularly comprises the following steps: dissolving cefalotin acid into an organic acid, carrying out carboxyl protection by using a silanization protection reagent and then carrying out iodination reaction on reaction products and iodotrimethylsilane; then carrying out amination reaction on the reaction product from the former step and pyrazinamide; and finally carrying out deprotection by alcoholysis, regulating the pH value at a low temperature and crystalizing to obtain cefalonium. According to the preparation method of cefalonium, cefalotin acid is protected by the silanization protection reagent in an organic solvent and then reacts with iodotrimethylsilane; the reaction time is short, the reaction conditions are mild, the reaction is complete and no side reaction is almost generated; due to adoption of a mixed solvent crystallization method, the characteristics of high drying speed, light color and high yield can be achieved; in addition, the used solvent can be recycled and the amount of generated sewage can be reduced; therefore, the preparation method of cefalonium has remarkable economic and environmental benefits and facilitates industrial production.

The invention discloses a preparation method of iodotrimethylsilane, which comprises: adding anhydrous aluminum chloride and hexamethyldisiloxane into a reaction vessel in the presence of a protective gas, starting to stir, and raising the temperature to 40‑50°C, then add iodine elemental substance, after the addition of iodine elemental substance, the bath temperature rises to 125‑140°C, and the reaction is refluxed for 1‑1.5 hours. Methyl iodosilane. The method can improve the yield of iodotrimethylsilane, has simple purification, mild conditions, and is suitable for large-scale production and popularization.