反应详情

A solution of the product of example 1 step a) (5.0 g), diisopropylethylamine (2.8 ml) and bromoacetonitrile (1.1 ml) in DMSO (50 ml) was heated at 100° C. for 5 hours. After cooling, the reaction mixture was partitioned between ethyl acetate and saturated aqueous ammonium chloride. The organic phase was dried over magnesium sulphate, filtered and evaporated to give a black oil which was purified by silica gel flash column chromatography, eluting with 10:1 dichloromethane:ethyl acetate, to give the subtitled compound as a pale orange solid (1.6 g).

1. temperatureAfter cooling
2. customthe reaction mixture was partitioned between ethyl acetate and saturated aqueous ammonium chloride
3. dry with materialThe organic phase was dried over magnesium sulphate
4. filtrationfiltered
5. customevaporated
6. customto give a black oil which
7. customwas purified by silica gel flash column chromatography
8. washeluting with 10:1 dichloromethane