反应详情

温度

40 °C

A mixture of (3-methyl-4-(methyl(7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)amino)cyclohexyl)methanesulfonic acid (0.400 g, 0.81 mmol), CH2Cl2 (10 mL), and DMF (50 uL) was treated with thionyl chloride and warmed to 40° C. After 1.5 h, the mixture was cooled, treated with toluene (5 mL) and concentrated. The resulting material was triturated with Et2O and dried to afford (3-methyl-4-(methyl(7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)amino)cyclohexyl)methanesulfonyl chloride that was used immediately without additional manipulation. MS for C22H27ClN4O4S2 (ESI) (MH)+ m/z=512.

1. temperaturethe mixture was cooled
2. concentrationconcentrated
3. customThe resulting material was triturated with Et2O
4. customdried