反应详情

Me2S complex (2M in THF) (20 eq) was added to a stirred solution of methyl 4-(acetylamino)-13-cyclohexyl-6-oxo-6,7-dihydro-5H-indolo[1,2-d][1,4]benzodiazepine-10-carboxylate in anhydrous THF (0.02 M) at RT under N2. After 45 min further BH3.Me2S complex (2M in THF) (5 eq) were introduced and the reaction left to stir for 1 h. The reaction was quenched by cautious addition of 1N HCl (aq) and MeOH before partitioning between saturated NaHCO3 (aq) and EtOAc. The organics were washed with water, brine before being dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to afford the crude product. Purification by flash chromatography (3% MeOH/CH2Cl2) afforded the title compound (36%). MS (ES+) m/z 414 (M+H)+.

1. waitthe reaction left
2. customThe reaction was quenched by cautious addition of 1N HCl (aq) and MeOH
3. custombefore partitioning between saturated NaHCO3 (aq) and EtOAc
4. washThe organics were washed with water, brine
5. dry with materialbefore being dried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customto afford the crude product
9. customPurification by flash chromatography (3% MeOH/CH2Cl2)