反应详情

1.30 g (4.76 mmol) of 4-(1H-pyrrolo[2,3-b]pyridin-3-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid ethyl ester were dissolved in 11 ml of DMF and, at room temperature, 0.25 g (5.6 mmol) of 60% sodium hydride were carefully added. This mixture was stirred for half an hour at room temperature. 0.75 ml (6.0 mmol) of 2-bromoethyl ethyl ether were dropwise added and the stirring was continued for 24 hours at 60° C. The reaction mixture was cooled to room temperature and poured over cold water. This aqueous phase was extracted twice with dichloromethane and the organic phase was washed with water and brine, dried with magnesium sulphate, filtered and evaporated to dryness. The 1.46 g (74% of yield) of crude material were pure enough for the next synthetic step.

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionThis aqueous phase was extracted twice with dichloromethane
3. washthe organic phase was washed with water and brine
4. dry with materialdried with magnesium sulphate
5. filtrationfiltered
6. customevaporated to dryness
7. customThe 1.46 g (74% of yield) of crude material