反应详情

A mixture of 1.35 g of 1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one and 15 ml of tert-butoxy-bis(dimethylamino)methane is heated for on a steam bath for 2 hours. The volatiles are evaporated in vacuo to a residue which is stirred with ether and filtered. The cake is washed with ether and the combined filtrates evaporated in vacuo to a residue which is dissolved in 30% ethyl acetate in methylene chloride and passed through a pad of hydrous magnesium silicate. The filtrate is evaporated in vacuo to a residue which is dissolved in 30% ethyl acetate in methylene chloride and passed through a pad of hydrous magnesium silicate. The filtrate is evaporated in vacuo to a residue to give 1.60 g of yellow crystalline product, m.p. 180°-183° C.

1. temperatureis heated for on a steam bath for 2 hours
2. customThe volatiles are evaporated in vacuo to a residue which
3. filtrationfiltered
4. washThe cake is washed with ether
5. customthe combined filtrates evaporated in vacuo to a residue which
6. dissolutionis dissolved in 30% ethyl acetate in methylene chloride
7. customThe filtrate is evaporated in vacuo to a residue which
8. dissolutionis dissolved in 30% ethyl acetate in methylene chloride
9. customThe filtrate is evaporated in vacuo to a residue