HRID1435735

反应详情

EQUATION

反应方程式

HRID 1435735 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,4-dichloro-6-(5-chloro-2-methyl-phenyl)-[1,3,5]triazine (2.5 g, 9.1 mmol), 4-bromoaniline (1.6 g, 9.3 mmol), tetrahydrofuran (60 ml), and diisopropylethylamine (1.6 ml, 9.2 mmol) was stirred for 1 hour. The solution was treated with dichloromethane (200 ml), washed with saturated aqueous sodium chloride solution (50 ml), and concentrated under reduced pressure. The residual solid was treated with hydrochloric acid (1 M, 25 ml) and stirred vigorously for 30 minutes. Filtration and drying under reduced pressure provided the title compound (3.2 g, 86% yield). 1H NMR (DMSO-d6) 10.75-10.80 (m, 1H), 7.85-7.92 (m, 1H), 7.50-7.65 (m, 4H), 7.40 (m, 1H), 2.58 (s, 3H).

WORKUP

后处理

  1. washwashed with saturated aqueous sodium chloride solution (50 ml)
  2. concentrationconcentrated under reduced pressure
  3. additionThe residual solid was treated with hydrochloric acid (1 M, 25 ml)
  4. stirringstirred vigorously for 30 minutes
  5. filtrationFiltration
  6. customdrying under reduced pressure