HRID1156886

反应详情

EQUATION

反应方程式

HRID 1156886 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-20 °C

PROCEDURE

实验过程

One hundred and fifty (150) grams of methyl 2-cyanomethylbenzoate ("Yakugaku Zasshi", Vol. 86, p. 544, 1966) was added dropwise to a suspension of 60 g of lithium aluminum hydride and 211 g of aluminium chloride in ether while maintaining the suspension at -20° C. The mixture was stirred at room temperature for 5 hours, and the aluminum complex was decomposed with 520 ml of a 10 N aqueous solution of sodium hydroxide and 140 ml of water. The residue was extracted with tetrahydrofuran, dried, and distilled under reduced pressure to afford 45 g of 1-amino-2-(2-hydroxymethylphenyl)ethane as a colorless oil having a boiling point of 125° C./0.5 mmHg.

WORKUP

后处理

  1. extractionThe residue was extracted with tetrahydrofuran
  2. customdried
  3. distillationdistilled under reduced pressure