反应详情

温度

110 °C

The intermediate 1A (6.0 g; 20.8 mmol) in solution in xylene (76 ml), under nitrogen, is treated with trimethyltin azide (6.25 g; 31.3 mmol). After stirring for 24 h at 110° C., the reaction medium is brought to room temperature and the precipitate formed is filtered on sintered glass and then washed with toluene and with petroleum ether. This solid is purified by chromatography on a silica gel column eluted with a dichloromethane/methanol/ammonium hydroxide mixture in the proportions 80/19/1 to give compound 1B (5.75 g; 87%) in the form of a white solid.

1. customis brought to room temperature
2. customthe precipitate formed
3. filtrationis filtered on sintered glass
4. washwashed with toluene and with petroleum ether
5. customThis solid is purified by chromatography on a silica gel column
6. washeluted with a dichloromethane/methanol/ammonium hydroxide mixture in the proportions 80/19/1