Intermediate of telmisartan, preparation and use thereof
A technology for telmisartan and intermediates, applied in the field of preparation of telmisartan, can solve the problems of short reaction time, small environmental pollution, serious environmental pollution, etc., and achieve the advantages of industrial production, small environmental pollution and safe operation Effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0040] Example 1: Preparation of 7-methyl-2-propyl-3H-benzimidazole-5-carbonyl chloride
[0041] In a 250ml there-necked flask, add 11g of 7-methyl-2-propyl-3H-benzimidazole-5-carboxylic acid, 100ml of thionyl chloride and 1ml of DMF, heat to reflux under stirring for half an hour, and recover excess chlorine under reduced pressure Sulfoxide was dissolved, 100 ml of toluene was added, stirred and filtered to dryness to obtain 7-methyl-2-propyl-3H-benzimidazole-5-carbonyl chloride, which was directly used in the next step.
Embodiment 2
[0042] Example 2: Preparation of 7-methyl-N-(2-(methylamino)phenyl)-2-n-propyl-3H-benzimidazole-5-carboxamide
[0043] In a 500ml three-necked flask, 9.5g of N-methyl-o-phenylenediamine hydrochloride and 300ml of dichloromethane were added, stirred and cooled to between 0 and 5°C, and benzimidazole acid chloride obtained in the previous step was added. Triethylamine was added dropwise at a temperature, and stirring was continued for half an hour after the dropwise addition, the reaction solution was suction filtered, the filtrate was concentrated to dryness, the residue was dissolved in 300 ml of 5% dilute hydrochloric acid, and 5% sodium hydroxide solution was used under stirring. The pH value of the solution was adjusted to 11, a white solid was precipitated, suction filtered, the filter cake was washed with water until neutral, and dried to constant weight under an infrared lamp to obtain 7-methyl-N-(2-(methylamino)phenyl) -2-n-propyl-3H-benzimidazole-5-carboxamide, yield 8...
Embodiment 3
[0044] Example 3: 4'-((4-methyl-6-(2-methylamino)phenylcarbamoyl)-2-n-propyl-1H-benzimidazol-1-yl)methyl)biphenyl - Preparation of methyl 2-carboxylate
[0045] Add 7-methyl-N-(2-(methylamino)phenyl)-2-n-propyl-3H-benzimidazole-5-carboxamide 10g, 300ml acetonitrile in a 500ml there-necked flask with nitrogen protection, Stir and cool to between 0~5 ℃, add 4g of sodium hydride and stir for 10 minutes, add 9g of 4'-bromomethylbiphenyl-2-carboxylic acid benzyl ester in batches under insulation, continue to stir for half an hour after the addition, the reaction The liquid was poured into 500 ml of water, the aqueous phase was extracted with dichloromethane, the dichloromethane layers were combined, and concentrated to dryness to obtain 4'-((4-methyl-6-(2-methylamino)phenylcarbamoyl)-2 - n-propyl-1H-benzimidazol-1-yl)methyl)biphenyl-2-carboxylate methyl ester. Yield 62%.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 