HRID4258

反应详情

EQUATION

反应方程式

HRID 4258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred 0° C. solution of the resultant compound of Example 5 (79 mg, 0.23 mmol) in dry THF (8 ml) was added vinyl magnesium bromide (1.5 ml of a 1.0M solution in THF) dropwise. The mixture was warmed (room temperature, 10 hours), quenched (8 ml H2O+2 ml brine), acidified with 0.1M H3PO4 (pH=7), and extracted with ether (3×4 ml). The combined ether phase was washed (4 ml brine), dried (Na2SO4), filtered, and evaporated to give 81 mg (95%) of the desired product as a 4:1 mixture of diastereomers.

WORKUP

后处理

  1. customquenched (8 ml H2O+2 ml brine)
  2. extractionextracted with ether (3×4 ml)
  3. washThe combined ether phase was washed (4 ml brine)
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated