HRID861220

反应详情

EQUATION

反应方程式

HRID 861220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

3-amino-phenylacetic acid benzyl ester p-toluene sulphonic acid was prepared by adding 3-aminophenylacetic acid (10 g) and p-toluene sulphonic acid monohydrate (13.2 g) to benzyl alcohol (27.2 ml) in toluene (30 ml). The mixture was heated under reflux and the water formed collected in a Dean-Stark receiver. When all the rarer had been distilled off the mixture was allowed to cool to 25° C. before diluting with diethyl ether and placing in an ice-bath for 1 hr. The crystalline p-toluene sulphonate was filtered off and dried in a dissicator (23.5 g) NMR δ2.31(s)3H, 3.82(s)2H, 5.11(s)2H, 7.11(d)2H, 7.25-7.45(m)8H, 7.52(d)2H.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux
  3. customcollected in a Dean-Stark receiver
  4. distillationWhen all the rarer had been distilled off the mixture
  5. additionbefore diluting with diethyl ether
  6. filtrationThe crystalline p-toluene sulphonate was filtered off
  7. customdried in a dissicator (23.5 g) NMR δ2.31(s)3H, 3.82(s)2H, 5.11(s)2H, 7.11(d)2H, 7.25-7.45(m)8H, 7.52(d)2H