HRID486487

反应详情

EQUATION

反应方程式

HRID 486487 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Lithium diisopropylamide (3.67 ml of a 1.5 molar solution in cyclohexane) was added to acetonitrile (0.26 ml) in tetrahydrofuran (10 ml) at -78° C. After 1 hour, methyl 2-phenyl-acrylate (see Preparation 22) (0.81 g) in tetrahydrofurn (10 ml) was added and the mixture was stirred for 1 hour, allowed to warm to room temperature then treated with saturated ammonium chloride solution. The resulting mixture was partitioned between ethyl acetate and water, the organic phase dried over magnesium sulphate and evaporated to give a residue which was partitioned between ether and 10% aqueous sodium carbonate. The organic layer was dried over magnesium sulphate and evaporated to leave the title compound (0.5 g, 75%) as an oil.

WORKUP

后处理

  1. customThe resulting mixture was partitioned between ethyl acetate and water
  2. dry with materialthe organic phase dried over magnesium sulphate
  3. customevaporated
  4. customto give a residue which
  5. customwas partitioned between ether and 10% aqueous sodium carbonate
  6. dry with materialThe organic layer was dried over magnesium sulphate
  7. customevaporated