HRID4588

反应详情

EQUATION

反应方程式

HRID 4588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Cyano-2(R,S)-α-naphthylmethylbutyric acid: 2.13 g of 2-cyanoethylmalonic acid diethyl ester are added to a suspension of 0.48 g of sodium hydride dispersion in 25 ml of DMF. The reaction mixture is stirred for 2 hours at 80° and then, at room temperature, 1.77 g of α-chloromethylnaphthalene in 5 ml of DMF are added. The mixture is further stirred for 16 hours at 50° and then concentrated by evaporation. The residue is dissolved in ethyl acetate, washed with 0.1N hydrochloric acid and water, dried over sodium sulphate and concentrated by evaporation, leaving 2-cyanoethyl-α-naphthylmethylmalonic acid diethyl ester.

WORKUP

后处理

  1. stirringThe mixture is further stirred for 16 hours at 50°
  2. concentrationconcentrated by evaporation
  3. dissolutionThe residue is dissolved in ethyl acetate
  4. washwashed with 0.1N hydrochloric acid and water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated by evaporation