Reacción #48275

Ecuación de reacción

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

hydrogen

→

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

Rendimiento 113.4%

Disolventes

triethylamine

methanol

Condiciones de reacción

Tratamiento posterior

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

Procedimiento

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.

Fuente