反应详情

温度

55 °C

To a solution of 0,50 g of 6,7-dihydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine in 10 ml of ethyl alcohol and 2 ml of tetrahydrofuran is added 2.35 g of SnCl2.2H2O and the mixture stirred at 55° C. for 30 minutes. The solvents are evaporated in vacuo to a residue which is stirred with 20 ml of 1N NaOH and 40 ml of ethyl acetate for 15 minutes and filtered through diatomaceous earth. The filter pad is washed with 2×10 ml of ethyl acetate and the combined extracts washed with brine, dried (Na2SO4) and evaporated in vacuo to give 0.47 g of solid residue which is triturated with ether-hexane to give 0.43 g of light yellow crystalline solid. MS(CI): 338 (M+H, Cl35) 340 (M+H, Cl37)

1. customThe solvents are evaporated in vacuo to a residue which
2. stirringis stirred with 20 ml of 1N NaOH and 40 ml of ethyl acetate for 15 minutes
3. filtrationfiltered through diatomaceous earth
4. washThe filter pad is washed with 2×10 ml of ethyl acetate
5. washthe combined extracts washed with brine
6. dry with materialdried (Na2SO4)
7. customevaporated in vacuo