HRID2383129

反应详情

EQUATION

反应方程式

HRID 2383129 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, 21 mL, 0.25 mol) was added to a suspension of 6-benzyloxy-4-chloro-3-nitroquinoline (13.74 g, 43.65 mmol) 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 three hours. A precipitate formed, which was isolated by filtration, washed with distilled water (3×), and recrystallized from 2-propanol (44.2 mL/g). The crystals were isolated by filtration and washed with cold hexanes (2×100 mL) to provide 11.36 g of N-(6-benzyloxy-3-nitroquinolin-4-yl)-N-methylamine as orange crystals.

WORKUP

后处理

  1. temperatureto cool to ambient temperature
  2. stirringstirred for three hours
  3. customA precipitate formed
  4. customwhich was isolated by filtration
  5. washwashed with distilled water (3×)
  6. customrecrystallized from 2-propanol (44.2 mL/g)
  7. customThe crystals were isolated by filtration
  8. washwashed with cold hexanes (2×100 mL)