反应详情

A solution of 0.150 g of 4-[(dimethylamino)methylene]-1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one and 44 μl of methylhydrazine in 5 ml of methyl alcohol is heated at reflux for 18 hours. A precipitate forms on standing. The volatiles are evaporated to a residue which is purified by column chromatography on silica gel by elution with 5% ethyl acetate-methylene chloride. The product fractions are combined and the volatiles evaporated to a residue which is dissolved in chloroform-methanol, filtered through glass wool and the filtrate evaporated in vacuo to give 0.110 g of the desired product as pale yellow crystals.

1. temperatureat reflux for 18 hours
2. customThe volatiles are evaporated to a residue which
3. customis purified by column chromatography on silica gel by elution with 5% ethyl acetate-methylene chloride
4. customthe volatiles evaporated to a residue which
5. dissolutionis dissolved in chloroform-methanol
6. filtrationfiltered through glass wool
7. customthe filtrate evaporated in vacuo