反应详情

2,3-Difluorophenylacetyl chloride(58.1 mmol) in CH2Cl2 (150 ml)was added to a suspension of 5-bromo-1H-pyrrolo[2,3-b]pyridine (8.0 g, 40.6 mmol) and AlCl3 (46 g, 345 mmol) in CH2Cl2 (100 ml) at 0° C. After the addition, the cooling bath was removed and the reaction mixture was stirred at room temperature for 1.5 hrs. The reaction was cooled with ice-bath and methanol (100 ml) was added to the reaction mixture while maintaining the temperature below 30° C. The reaction mixture was evaporated and the residue was suspended in water. The solid was collected by vacuum filtration, washed with water and hexane to give the title compound (14.03 g) in 98% yield.

1. additionAfter the addition
2. customthe cooling bath was removed
3. temperatureThe reaction was cooled with ice-bath
4. additionmethanol (100 ml) was added to the reaction mixture
5. temperaturewhile maintaining the temperature below 30° C
6. customThe reaction mixture was evaporated
7. filtrationThe solid was collected by vacuum filtration
8. washwashed with water and hexane