反应详情

温度

0 °C

A solution of 0.79 ml (10 mmol) thionylchloride in 5.5 ml of toluene is cooled to −10° C. Solid {4-[4-(3-chloro-benzylamino)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-phenyl}-methanol is added and the suspension stirred at 0° C. for 2 h and then at RT for 17 h. The solid is filtered off, washed with toluene and suspended in water (3 ml). The mixture is treated with saturated sodium bicarbonate solution (3 ml) and stirred for 10 min. The crystals are collected by filtration washed with water, a small amount of ethanol and ether and dried to give the title compound; m.p. decomposition ˜300° C.; Rf(dichloromethane/methanol/conc. ammonia 90:10:1)=0.61; MS-ES+: (M+H)+=383.

1. waitat RT for 17 h
2. filtrationThe solid is filtered off
3. washwashed with toluene
4. additionThe mixture is treated with saturated sodium bicarbonate solution (3 ml)
5. stirringstirred for 10 min
6. filtrationThe crystals are collected by filtration
7. washwashed with water
8. dry with materiala small amount of ethanol and ether and dried