HRID53532

反应详情

EQUATION

反应方程式

HRID 53532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of N-(2-bromo-6-methoxy-4-methyl-3-pyridinyl)-2-chloro-3-pyridinecarboxamide (2.1 g), dioxane (10 ml), and ethylamine (0.5 g) was heated to 140° C. in a sealed tube for 5 hours. The cooled mixture was diluted with ethyl acetate, washed with water, and the organic phase was dried (anhydrous magnesium sulfate) and concentrated. The product was purified on a silica gel column (methylene chloride/ethyl acetate, 99:1) and crystallized by trituration with diisopropyl ether to give 0.95 g of the title compound.

WORKUP

后处理

  1. washwashed with water
  2. dry with materialthe organic phase was dried (anhydrous magnesium sulfate)
  3. concentrationconcentrated
  4. customThe product was purified on a silica gel column (methylene chloride/ethyl acetate, 99:1)
  5. customcrystallized by trituration with diisopropyl ether