反应详情

A mixture of 0.780 g of 1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one and 10 ml of tert-butoxy bis(dimethylamino)methane (Bredereck's Reagent) is heated on a steam bath while stirring for 1.5 hours (solid dissolved). Cooling gives a solid and the mixture is diluted with ethyl acetate and filtered. The solid is dissolved in dichloromethane-ethyl acetate (7:3) and the solution filtered through a thin pad of hydrous magnesium silicate. The filter pad is washed with dichloromethane-ethyl acetate (7:3) and the combined filtrate evaporated to give 0.43 g of yellow crystals, Mass Spec (CI) MH+ =366, m.p. 180°-183° C.

1. temperatureis heated on a steam bath
2. dissolution(solid dissolved)
3. temperatureCooling
4. customgives a solid
5. filtrationfiltered
6. dissolutionThe solid is dissolved in dichloromethane-ethyl acetate (7:3)
7. filtrationthe solution filtered through a thin pad of hydrous magnesium silicate
8. washThe filter pad is washed with dichloromethane-ethyl acetate (7:3)
9. customthe combined filtrate evaporated