反应详情

Combine (S)-2-chloro-11-[3-(2-methoxy-ethyl)-piperazin-1-yl]-5H-dibenzo[b,e][1,4]diazepine (0.474 g, 1.27 mmol) and 37% formaldehyde solution (0.1 mL, 1.34 mmol) in 1,2-dichloroethane (20 mL). Stir for 10 minutes and add sodium triacetoxy borohydride (0.542 g, 2.55 mmol). Stir an additional 30 minutes and then pour solution onto saturated sodium bicarbonate solution. Extract with methylene chloride to give 0.555 g of the crude product. Silica gel chromatography, eluting with methylene chloride:methanol (100:5), gives 0.490 g of the title compound as the free base. The dihydrochloride salt precipitates in ethyl acetate as a solid: mp 205° C.; mass spectrum (ion spray): m/z=385 (M+1).

1. stirringStir an additional 30 minutes
2. extractionExtract with methylene chloride
3. customto give 0.555 g of the crude product
4. washSilica gel chromatography, eluting with methylene chloride:methanol (100:5)