반응 #48275

반응 방정식

6-(Chloro-difluoro-methyl)-2-(3-methoxy-propyl)-nicotinic acid methyl ester

hydrogen

→

6-Difluoromethyl-2-(3-methoxy-propyl)-nicotinic acid methyl ester

수율 113.4%

용매

triethylamine

methanol

반응 조건

후처리

1. 1
   여과After completion of the reduction the reaction mixture is filtered through hyflo
2. 2
   workup.ADDITIONthe filtrate diluted with water
3. 3
   추출the water/methanol mixture then extracted with ethyl acetate
4. 4
   세척The combined ethyl acetate extracts are washed with saturated aqueous sodium chloride solution
5. 5
   건조dried over magnesium sulphate
6. 6
   농축concentrated in vacuo

실험 절차

A solution of 194 g of 6-(Chloro-difluoro-methyl)-2-(3-methoxy-propyl)-nicotinic acid methyl ester (prepared according to WO 04/078729) in methanol (ca. 2 liter) and triethylamine (100 ml) is hydrogenated at 1 Atm hydrogen pressure in the presence of 2 g of 5% palladium supported on carbon. After completion of the reduction the reaction mixture is filtered through hyflo, and the filtrate diluted with water and the water/methanol mixture then extracted with ethyl acetate. The combined ethyl acetate extracts are washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate and then concentrated in vacuo to give 194.2 g 6-Difluoromethyl-2-(3-methoxy-propyl)-nicotinic acid methyl ester as a pale coloured oil.

출처