反应详情

2-{4-(1,3-Benzodioxol-5-yl)-5-methoxy-3-[(methoxymethyl)(phenethylsulfonyl)amino]-1H-pyrazol-1-yl}ethyl acetate (Preparation 54) (70 mg), oxalic acid (200 mg) were dissolved in a mixture of water (2 ml) and methanol (2 ml) and refluxed for two days. The reaction was diluted with water (10 ml) and the mixture was then extracted with dichloromethane (3×8 ml). The combined organic fractions were dried over sodium sulfate, concentrated under reduced pressure to yield a pale yellow oil which was purified by column chromatography (Sep-Pak™, 10 g) eluted with dichloromethane:methanol (97:3) to yield the title compound as a colourless oil (32 mg).

1. temperaturerefluxed for two days
2. extractionthe mixture was then extracted with dichloromethane (3×8 ml)
3. dry with materialThe combined organic fractions were dried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customto yield a pale yellow oil which
6. customwas purified by column chromatography (Sep-Pak™, 10 g)
7. washeluted with dichloromethane:methanol (97:3)