反应详情

The Boc-protected piperazine from step A (1.5 g, 4.5 mmol) was added to a 1:1 mixture of trifluoroacetic acid and dichloromethane (10 ml). The reaction was stirred overnight, then concentrated under vacuum, diluted with dichloromethane, and neutralized with sat. aq. sodium bicarbonate. The layers were separated, and the aqueous layer was back extracted with more dichloromethane. The combined organic fractions were dried over MgSO4 and concentrated under vacuum to give (S)-5-methyl-4-(3-methylpiperazin-1-yl)-7H-pyrrolo[2,3-d]pyrimidine (0.80 g, 3.5 mmol, 76%).

1. concentrationconcentrated under vacuum
2. additiondiluted with dichloromethane
3. customThe layers were separated
4. extractionthe aqueous layer was back extracted with more dichloromethane
5. dry with materialThe combined organic fractions were dried over MgSO4
6. concentrationconcentrated under vacuum