HRID1735143
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
- 80 °C
PROCEDURE
实验过程
In 9 ml of N-methylpyrrolidone, was dissolved 3.9 g of the compound obtained in Example 38, and 2.64 g of urea was further added thereto. The reaction was carried out at 160° C. for one hour. The reaction mixture was cooled to 80° C. and 100 ml of water was added. The precipitated crystals were collected by filtration and dissolved in a mixture of 5 ml of methanol and 150 ml of chloroform. The solution was dried over anhydrous sodium sulfate and evaporated to dryness. The obtained product was recrystallized from ethanol-ethyl acetate to obtain 2.44 g of the titled compound having the melting point of 260° to 263° C.
WORKUP
后处理
- additionwas further added
- filtrationThe precipitated crystals were collected by filtration
- dissolutiondissolved in a mixture of 5 ml of methanol and 150 ml of chloroform
- dry with materialThe solution was dried over anhydrous sodium sulfate
- customevaporated to dryness
- customThe obtained product was recrystallized from ethanol-ethyl acetate