HRID1373948

反应详情

EQUATION

反应方程式

HRID 1373948 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A suspension of tert-butyl N′-(7-bromo-3-nitroquinolin-4-yl)hydrazinecarboxylate (50.0 g, 131 mmol) in 320 mL of acetonitrile (MeCN) and 80 mL of methanol was treated with platinum on carbon (5.0 g, 1.3 mmol, 5% w/w) and shaken under an atmosphere of hydrogen (3.8×105 Pa). After 4 h, the reaction mixture was filtered through a pad of CELITE filter agent and rinsed with portions of MeCN:MeOH (1:1) until the filtrate ran clear. The filtrate was concentrated under reduced pressure to yield 37.1 g of tert-butyl N′-(3-amino-7-bromoquinolin-4-yl)hydrazinecarboxylate as a tan solid.

WORKUP

后处理

  1. filtrationthe reaction mixture was filtered through a pad of CELITE
  2. filtrationfilter agent
  3. washrinsed with portions of MeCN:MeOH (1:1) until the filtrate
  4. concentrationThe filtrate was concentrated under reduced pressure