HRID1534834

反应详情

EQUATION

反应方程式

HRID 1534834 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 35.28 g (105.5 mmole) methyl (triphenylphosphoranylidene)acetate in 70 mL methylene chloride was added to a solution of 11.36 g (52.76 mmoles) of (7) in 20 mL methylene chloride. After 2 h at room temperature, the solution was concentrated in vacuo to remove most of the solvent and the residue was diluted with ether. The solid was removed by filtration and the filtrate was concentrated and the residue chromatographed (Flash, hexane-ethyl acetate 7:3). The product fraction amounted to 10.7 g of a colorless oil (8).

WORKUP

后处理

  1. concentrationthe solution was concentrated in vacuo
  2. customto remove most of the solvent
  3. additionthe residue was diluted with ether
  4. customThe solid was removed by filtration
  5. concentrationthe filtrate was concentrated
  6. customthe residue chromatographed (Flash, hexane-ethyl acetate 7:3)