反应详情

A solution of the product of stage (ii) in methylacetate (5 ml) was treated with ethereal hydrogen chloride (5 ml). The resulting solid was collected by filtration and added to thionyl chloride (7.5 ml) at 0°-5°. The mixture was stirred at 0°-5° for 3 h and then at ambient temperature for 1 h. Diethyl ether (100 ml) was added and the resulting solid was collected by filtration and washed with diethylether (2×50 ml), to give the title compound as a solid (1.7 g) T.l.c. Silica dichloromethane/methanol/ammonia 75:10:2 Rf 0.8.

1. filtrationThe resulting solid was collected by filtration
2. additionadded to thionyl chloride (7.5 ml) at 0°-5°
3. waitat ambient temperature for 1 h
4. additionDiethyl ether (100 ml) was added
5. filtrationthe resulting solid was collected by filtration
6. washwashed with diethylether (2×50 ml)