反应详情

A mixture of 400 mg of 6,7-dihydro-2-methyl-7-(4-nitrobenzoyl)-5H-pyrimido[5,4-d][l]benzazepine, 87 μl of anhydrous hydrazine and 40 mg of 10% Pd/C in 22 ml of ethyl alcohol is heated at reflux for 1.25 hours, filtered through diatomaceous earth and the pad washed well with methyl alcohol. The combined filtrates are evaporated in vacuo to a residue which is dissolved in ethyl acetate and filtered through a pad of hydrous magnesium silicate and the filtrate concentrated in vacuo to a residue which is dissolved in methyl alcohol and evaporated again to give 330 mg of the desired product as a yellow foam. HR FABMS: Exact mass (M+H): 331.1555.

1. temperatureis heated
2. temperatureat reflux for 1.25 hours
3. filtrationfiltered through diatomaceous earth
4. washthe pad washed well with methyl alcohol
5. customThe combined filtrates are evaporated in vacuo to a residue which
6. dissolutionis dissolved in ethyl acetate
7. filtrationfiltered through a pad of hydrous magnesium silicate
8. concentrationthe filtrate concentrated in vacuo to a residue which
9. dissolutionis dissolved in methyl alcohol
10. customevaporated again