反应详情

A mixture of 9-(2-methanesulfonyloxyethyl)-2,4-di-1-pyrrolidinyl-9H-pyrimido[4,5-b]indole (IX, EXAMPLE 4, 1.3 g) and 15 ml of ethanolamine is heated to reflux for 4 hr, then cooled, and diluted with methylene chloride (100 mL) and aqueous saturated sodium bicarbonate. The phases are separated, and the aqueous phase is extracted again with methylene chloride/chloroform (1/1). The combined extracts are dried over sodium sulfate and concentrate under reduced pressure at 50°-60° to give a solid. The solid is recrystallized from ethyl acetate/hexane at 20°-250 to give the title compound, NMR (CDCl3) 1.5-1.7, 1.9-2.0, 2.84, 3.12, 3.56, 3.63, 3.92, 4.20, 7.10, 7.13-7.30 and 7.80 δ; MS (EI, m/z) 394 (M+), 363, 320 and 307.

1. temperatureis heated
2. temperatureto reflux for 4 hr
3. temperaturecooled
4. customThe phases are separated
5. extractionthe aqueous phase is extracted again with methylene chloride/chloroform (1/1)
6. dry with materialThe combined extracts are dried over sodium sulfate
7. concentrationconcentrate under reduced pressure at 50°-60°
8. customto give a solid
9. customThe solid is recrystallized from ethyl acetate/hexane at 20°-250