HRID1534834
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationthe solution was concentrated in vacuo
- customto remove most of the solvent
- additionthe residue was diluted with ether
- customThe solid was removed by filtration
- concentrationthe filtrate was concentrated
- customthe residue chromatographed (Flash, hexane-ethyl acetate 7:3)