反应详情

A mixture of 25 parts of 5-chloro-2-nitrobenzenemethanol, 13.3 parts of 3,4-dihydro-2H-pyran, 0.28 parts of dichloromethane and 300 parts of 4-methylbenzenesulfonic acid was stirred and for 2 hours at reflux temperature. After cooling, there was added Na2CO3 and the whole was stirred for 10 min. The reaction mixture was filtered and the filtrate was evaporated. The residue was co-evaporated with methylbenzene and was further purified by column chromatography (silica gel; CHCl3). The eluent of the desired fraction was evaporated and the residue was co-evaporated with methylbenzene, yielding 36 parts (99.6%) of 2-[(5-chloro-2-nitrophenyl)methoxy]-tetrahydro-2H-pyran (interm. 54).

1. temperatureat reflux temperature
2. temperatureAfter cooling
3. stirringthe whole was stirred for 10 min
4. filtrationThe reaction mixture was filtered
5. customthe filtrate was evaporated
6. customwas further purified by column chromatography (silica gel; CHCl3)
7. customThe eluent of the desired fraction was evaporated