反应详情

The mixture of 1-ethoxycarbonylmethyl-5-(4-nitrobenzoyl)-1,3,4,5-tetrahydro-1,5-benzodiazepin-2(2H)-one (667 mg), iron powder (469 mg), methanol (10 ml) and acetic acid (1 ml) was refluxed for 1 hour. The reaction mixture was cooled to ambient temperature and it was filtered through a bed of celite followed by the removal of methanol. The residue was diluted with chloroform and to the mixture was added saturated sodium bicarbonate aqueous solution followed by stirring for 10 minutes. The resulting mixture was filtered through a bed of celite and the organic layer was washed with brine. Drying the filtrate, and the removal of chloroform obtained a crude product. The crude product was triturated with a mixture of diisopropyl ether and n-hexane (1:1) to give 5-(4-aminobenzoyl)-1-ethoxycarbonylmethyl-1,3,4,5-tetrahydro-1,5-benzodiazepin-2(2H)-one (610 mg) as a slightly brown powder.

1. temperaturewas refluxed for 1 hour
2. filtrationit was filtered through a bed of celite
3. customfollowed by the removal of methanol
4. additionThe residue was diluted with chloroform and to the mixture
5. additionwas added saturated sodium bicarbonate aqueous solution
6. filtrationThe resulting mixture was filtered through a bed of celite
7. washthe organic layer was washed with brine
8. customDrying the filtrate
9. customthe removal of chloroform
10. customobtained a crude product
11. customThe crude product was triturated with a mixture of diisopropyl ether and n-hexane (1:1)