反应详情

A solution of the product from example 1, step (c) (0.12 g) and serinol (330 mg) in 1-methylimidazole (1 ml) was heated at 130° C. for 90 minutes. 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 brown solid which was purified by silica gel flash column chromatography, eluting with 200:20:1 dichloromethane:methanol:880 ammonia solution, to give the title compound as a pale brown solid (0.02 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 brown solid which
7. customwas purified by silica gel flash column chromatography
8. washeluting with 200:20:1 dichloromethane