HRID902994

反应详情

EQUATION

反应方程式

HRID 902994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

17.2 g (0.05 mole) of 4-(4'-trifluoromethylphenoxy)-α-phenoxypropionyl chloride are added dropwise at 10° C. to a mixture of 3.13 g (0.055 mole) of 100% hydroxyacetonitrile (cyanomethanol) and 5.5 g (0.54 mole) of triethylamine in 50 ml of methylene chloride. The reaction mixture is then stirred for 1 hour at room temperature. Then 100 ml of water are added and the organic phase is separated, filtered over a small column of silica gel and concentrated. The residual solid is triturated with petroleum ether, collected by filtration and dried, affording 13.2 g (72.5% of theory) of 4-(4'-trifluoromethylphenoxy)-α-phenoxy-propionic acid cyanomethyl ester with a melting point of 53°-56° C.

WORKUP

后处理

  1. customthe organic phase is separated
  2. filtrationfiltered over a small column of silica gel
  3. concentrationconcentrated
  4. customThe residual solid is triturated with petroleum ether
  5. filtrationcollected by filtration
  6. customdried