HRID324403

反应详情

EQUATION

反应方程式

HRID 324403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of the products from steps (viii) (0.65 g) and (ix) (1.025 g) and N,N-diisopropylethylamine (1.26 ml) in N-methylpyrrolidin-2-one (10 ml) was stirred at 90° C. for 24 hours. A further 0.342 g of product from step (ix) and N,N-diisopropylethylamine (0.5 ml) was added and heating continued for a further 24 hours. The solution was partitioned between 1N hydrochloric acid and ethyl acetate. The organic layer was washed with water, dried (MgSO4) and evaporated to give a brown oil which was purified by chromatography eluting with ethyl acetate.

WORKUP

后处理

  1. temperatureheating
  2. waitcontinued for a further 24 hours
  3. customThe solution was partitioned between 1N hydrochloric acid and ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customto give a brown oil which
  8. customwas purified by chromatography
  9. washeluting with ethyl acetate