HRID324414

反应详情

EQUATION

反应方程式

HRID 324414 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of the product from example 1 step (vi) (3.60 g) in tetrahydrofuran (30 ml) at −70° C. was treated dropwise with n-butyllithium (4.75 ml of a 2.5M solution in hexanes) and stirred for 30 minutes. A solution of the product from example 3 step (vi) (2.60 g) in tetrahydrofuran (30 ml) was added dropwise and the reaction stirred at room temperature for 3 hours. The reaction was partitioned between brine and ethyl acetate and the organics dried (MgSO4) and evaporation under reduced pressure gave a brown oil. Purification was by column chromatography eluting with 50% ethyl acetate in isohexane.

WORKUP

后处理

  1. stirringthe reaction stirred at room temperature for 3 hours
  2. customThe reaction was partitioned between brine and ethyl acetate
  3. customthe organics dried
  4. custom(MgSO4) and evaporation under reduced pressure
  5. customgave a brown oil
  6. customPurification
  7. washeluting with 50% ethyl acetate in isohexane