反应详情

A mixture of 3.24 g of 10,11-dihydro-10-(4-nitro-3-methoxybenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 0.35 g of 10% Pd/c and 0.60 g of anhydrous hydrazine in 100 ml of absolute ethyl alcohol and heated on a steam bath for 1 hour. The hot reaction mixture is filtered through diatomaceous earth and the filtrate evaporated in vacuo to a residue which is partitioned between methylene chloride and water. The organic layer is dried with Na2SO4 and passed through a short pad of hydrous magnesium silicate. Hexane is added to the filtrate while heating on a steam bath to give 2 g of crystals, m.p. 184°-185° C.

1. temperatureheated on a steam bath for 1 hour
2. filtrationThe hot reaction mixture is filtered through diatomaceous earth
3. customthe filtrate evaporated in vacuo to a residue which
4. customis partitioned between methylene chloride and water
5. dry with materialThe organic layer is dried with Na2SO4
6. additionHexane is added to the filtrate
7. temperaturewhile heating on a steam bath