HRID1789939

反应详情

EQUATION

反应方程式

HRID 1789939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the product from example 1, step (c) (0.25 g) and 2-amino-2-methyl-1,3-propanediol (0.28 ml) in N-methylimidazole (1 ml) was heated in a microwave at 160° C. for 95 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 oil which was purified by silica gel flash column chromatography, eluting with 10:1 dichloromethane:methanol to give the title compound as a pale brown solid (0.031 g).

WORKUP

后处理

  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 oil which
  7. customwas purified by silica gel flash column chromatography
  8. washeluting with 10:1 dichloromethane