HRID133785

反应详情

EQUATION

反应方程式

HRID 133785 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Step B (2): To a solution of 4-acetamido-3,5-dichloro-benzonitrile (114 mg, 0.5 mmol) in 5 mL of THF was added lithium aluminum hydride (120 mg, 3.2 mmol) in one portion and the resulting mixture was stirred for 3 h. Sodium sulfate decahydrate (1 g, 3.2 mmol) was added in one portion and the mixture was stirred for 30 min. The solid was filtered off and the filtrate was concentrated. The residue was purified by HPLC to give 4-acetamido-3,5-dichloro-benzylamine (35 mg, 30%). 1H NMR (500 MHz, CD3OD): δ 7.46 (s, 2 H), 3.78 (s, 2H), 2.18 (s, 3 H).

WORKUP

后处理

  1. stirringthe mixture was stirred for 30 min
  2. filtrationThe solid was filtered off
  3. concentrationthe filtrate was concentrated
  4. customThe residue was purified by HPLC