反应详情

To a mixture of 1-(2-methyl-3-difluoromethoxyphenyl)-4-methyl-1,4-dihydrotetrazole-5-one (described in Reference Preparation example 2) 1.0 g, 1,1′-azobis(cyclohexane-1-carbonitrile) 0.19 g, N-bromosuccinimide 0.80 g and chlorobenzene 50 ml was stirred with heating under reflux for eight hours. After cooling the mixture, to the reaction solutions was added water and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated saline, and was dried over anhydrous magnesium sulfate and was then concentrated under reduced pressure. The resulting residue was subjected to a silica gel column chromatography to give 1-(2-bromomethyl-3-difluoromethoxyphenyl)-4-methyl-1,4-dihydrotetrazole-5-one 1.1 g.

1. temperaturewith heating
2. temperatureunder reflux for eight hours
3. temperatureAfter cooling the mixture
4. extractionthe resulting mixture was extracted with ethyl acetate
5. washThe organic layer was washed with water and saturated saline
6. dry with materialwas dried over anhydrous magnesium sulfate
7. concentrationwas then concentrated under reduced pressure