HRID1088217
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe solution was evaporated
- customTrituration of the residue with chloroform:methanol (10:1) gave the crude product as a solid (0.78 g), m.p. 260°-270° C
- customThe filtrate was evaporated
- temperaturethe residue was heated at 180° C. for one hour
- customPurification of the residue by column chromatography (silica gel, chloroform:methanol, 25:1)