HRID2100466

反应详情

EQUATION

反应方程式

HRID 2100466 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

NaH (6.87 g, 172 mmol) was added slowly to a solution of 2-phenylethanol ([60-12-8], 6.00 g, 5.88 ml, 49.1 mmol) in DMF (50 ml). The reaction mixture was heated and kept for 10 min at 60° C. Chloroacetic acid ([79-11-8], 8.12 g, 86 mmol) was added slowly and carefully (exothermic), and the mixture was kept for 1 h at 60° C. The mixture was poured on ice and extracted twice with diethyl ether. Then the water phase was acidified (HCl, pH˜3) and extracted twice with ethyl acetate. Phenethyloxy-acetic acid [81228-03-7] was obtained after drying (Na2SO4), and evaporation of the solvent. The compound was sufficiently pure for the next step without further purification.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. waitcarefully (exothermic), and the mixture was kept for 1 h at 60° C
  3. additionThe mixture was poured on ice
  4. extractionextracted twice with diethyl ether
  5. extractionextracted twice with ethyl acetate