HRID1088217

反应详情

EQUATION

反应方程式

HRID 1088217 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A stirred mixture of 6-(4-aminophenyl)-5-methyl-4,5-dihydro-3(2H)-pyridazinone (3.25 g) and 5-methylthiouracil (2.5 g) was heated at 180° C. for 11/2 hours. The residual gum was dissolved in hot aqueous ethanol and the solution was evaporated. Trituration of the residue with chloroform:methanol (10:1) gave the crude product as a solid (0.78 g), m.p. 260°-270° C. The filtrate was evaporated and the residue was heated at 180° C. for one hour. Purification of the residue by column chromatography (silica gel, chloroform:methanol, 25:1) gave a further amount of product (0.73 g).

WORKUP

后处理

  1. customthe solution was evaporated
  2. customTrituration of the residue with chloroform:methanol (10:1) gave the crude product as a solid (0.78 g), m.p. 260°-270° C
  3. customThe filtrate was evaporated
  4. temperaturethe residue was heated at 180° C. for one hour
  5. customPurification of the residue by column chromatography (silica gel, chloroform:methanol, 25:1)