反应详情

温度

50 °C

A mixture of 0.91 g of 10,11-dihydro-10-(4-nitro-3-methoxybenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 4.51 g of SnCl2.2H2O, 6 ml of ethyl alcohol, 6 ml of tetrahydrofuran and 16 ml of methylene chloride is stirred at 50° C. for 2 hours. The solvents are evaporated in vacuo and the residue dissolved in 80 ml of ethyl acetate. The solution is treated with 50 ml of 1N NaOH with stirring for 30 minutes. The resulting suspension is filtered through diatomaceous earth. The pad is washed with ethyl acetate (3×15 ml). The combined ethyl acetate solutions are washed with brine, dried (Na2SO4), filtered through hydrous magnesium silicate and evaporated in vacuo to 0.99 g of residue which is stirred with ether-hexanes to give 0.90 g of cream colored solid. MS(CI): 334(M+H).

1. customThe solvents are evaporated in vacuo
2. dissolutionthe residue dissolved in 80 ml of ethyl acetate
3. additionThe solution is treated with 50 ml of 1N NaOH
4. stirringwith stirring for 30 minutes
5. filtrationThe resulting suspension is filtered through diatomaceous earth
6. washThe pad is washed with ethyl acetate (3×15 ml)
7. washThe combined ethyl acetate solutions are washed with brine
8. dry with materialdried (Na2SO4)
9. filtrationfiltered through hydrous magnesium silicate
10. customevaporated in vacuo to 0.99 g of residue which
11. stirringis stirred with ether-hexanes
12. customto give 0.90 g of cream