HRID900441

反应详情

EQUATION

反应方程式

HRID 900441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-60 °C

PROCEDURE

实验过程

To a solution of 2,4 dimethylthiazole (2 g) in dry tetrahydrofuran (20 ml) at −70° C. under argon was added 1.6M n-butyllithium in hexanes (12 ml) dropwise, keeping the temperature below −70° C. After stirring at −60° C. for 30 minutes, N-methoxy-N-methylacetamide (1.9 ml) was added. The mixture was allowed to warm to ambient temperature and was then partitioned between water and ethyl acetate The organic phase was dried (MgSO4) and the solvent removed under reduced pressure to yield a yellow oil. This was purified by column chromatography using a isohexane to 40% ethyl acetate/isohexane gradient as the eluent to yield the product as a yellow oil (630 mg, 23%).

WORKUP

后处理

  1. customthe temperature below −70° C
  2. temperatureto warm to ambient temperature
  3. customwas then partitioned between water and ethyl acetate The organic phase
  4. dry with materialwas dried (MgSO4)
  5. customthe solvent removed under reduced pressure
  6. customto yield a yellow oil
  7. customThis was purified by column chromatography