HRID1608776

反应详情

EQUATION

反应方程式

HRID 1608776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas further added
  2. filtrationThe precipitated crystals were collected by filtration
  3. dissolutiondissolved in a mixture of 5 ml of methanol and 150 ml of chloroform
  4. dry with materialThe solution was dried over anhydrous sodium sulfate
  5. customevaporated to dryness
  6. customThe obtained product was recrystallized from ethanol-ethyl acetate