Zhejiang Huahai Pharmaceutical Co., Ltd.

Zhejiang Jiuzhou Pharmaceutical Co., Ltd.

Min Li

Jinsheng Lin

Wenquan Zhu

Tianpei Huang

Peng Wang

Zhiyun Wang

Peng Dong

Hongjun Gao

Dan Li

Xiaoyan Xu

Wenbin Chen

Hong Cai

Tong Wu

Qiang Zhou

Yuanxun Zhu

Libin Hu

Tan Xiao

Danfeng Ye

Xiaoren Zhu

Feifei Lan

Xiaohui Zhou

Disclosed is N-formyl vortioxetine, and also disclosed is a method for preparing the N-formyl vortioxetine and a stable solid preparation of vortioxetine.

N-formyl vortioxetine and preparation method thereof and solid preparation of vortioxetine

Disclosed is a detection method for N-nitrosodimethylamine (NDMA) impurities, comprising: (1) obtaining a test solution containing a sample to be tested; and (2) detecting the test solution by means of gas chromatography-mass spectrometry to determine the content of an N-nitrosodimethylamine impurity in the sample. The method provided in the present invention has a good separating effect, a wide linear range, a high sensitivity and a good method durability, and can detect the content of N-nitrosodimethylamine (NDMA) in the sample rapidly and effectively.

Detection method for n-nitrosodimethylamine impurities

A method for synthesizing valsartan, comprising the steps of: synthesizing a valsartan methyl ester intermediate to obtain a reaction mixture of the valsartan methyl ester intermediate; diluting the reaction mixture by salt water or water, and then using a first extraction solvent to extract the valsartan methyl ester intermediate; adding alkali to an organic layer containing the valsartan methyl ester intermediate for hydrolyzing, removing the organic layer, regulating pH of a water layer to be acidic by using acid, using the first extraction solvent to extract, concentrating a part of solvent, or distilling the solvent to dryness, and then adding a new solvent; finally, crystallizing, filtering, and drying to obtain the valsartan.

Method for synthesizing valsartan

Sitagliptin intermediate compounds of formula (f) and methods of preparation and use thereof are disclosed. Compounds of formula (f) are prepared by the following steps: compounds of formula (a) are subjected to electrophilic reaction with benzyl halides to form compounds of formula (b), which then react with compounds of formula (i) to form novel compounds of formula (e). Gignard agents formed from 2,4,5-trifluoro bromobenzene and magnesium metal react with compounds of formula (e) to afford compounds of formula (f), which are novel intermediates for the preparation of Sitagliptin intermediates of formula (g). Compounds of formula (f) are subjected to reduction by Pd/C, debenzylation, substitution of protecting group to form compounds of formula (g). Compounds of formula (a), (b), (i), (e), (f), and (g) have the following structures, in which R is protecting group of carboxyl and Ris (substituted) hydrocarbyl. 

Sitagliptin intermediate compounds, preparation methods and uses thereof

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Taizhou, China

Min Li