HRID540844

反应详情

EQUATION

反应方程式

HRID 540844 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Methylamine (available as a 40% solution in water, 24 mL, 0.28 mol) was added to a solution of 6-benzyloxy-4-chloro-3-nitroquinoline (15.0 g, 48.5 mmol), prepared as described in Parts A-D of Example 2, in distilled water (300 mL), and the reaction was stirred at 100° C. for 1.5 hours. The reaction was allowed to cool to ambient temperature and stirred for four hours. A precipitate formed, which was isolated by filtration and washed with distilled water (3×60 mL). The solid was combined with material from another run and recrystallized from 2-propanol. The crystals were isolated by filtration, washed twice with cold hexanes, and dried for three days under high vacuum to provide 24.10 g of (6-benzyloxy-3-nitroquinolinyl)methylamine as yellow crystals.

WORKUP

后处理

  1. customprepared
  2. temperatureto cool to ambient temperature
  3. stirringstirred for four hours
  4. customA precipitate formed
  5. customwhich was isolated by filtration
  6. washwashed with distilled water (3×60 mL)
  7. customrecrystallized from 2-propanol
  8. customThe crystals were isolated by filtration
  9. washwashed twice with cold hexanes
  10. customdried for three days under high vacuum