HRID1417710

反应详情

EQUATION

反应方程式

HRID 1417710 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Amino-3-methyl-1-phenyl-2,4 (1H, 3H)-pyrimidinedione (5.00 g, 23 mmol) was suspended in dimethylformamide (77 mL). To the resultant suspension was added phosphorus oxychloride (2.57 mL, 27.6 mmol), and the resultant mixture was reacted at 60° C. for 3 h. The reaction mixture was diluted with water, and adjusted to ca. pH 12 with sodium hydroxide. The precipitates formed in the reaction mixture was filtered to give a crude product. The crude product was recrystallized from a mixture of ethanol, ethyl acetate and water to give an aldehyde, 6-amino-5-formyl-3-methyl-1-phenyl-2,4 (1H, 3H)-pyrimidinedione (yield 75%).

WORKUP

后处理

  1. customThe precipitates formed in the reaction mixture
  2. filtrationwas filtered
  3. customto give a crude product
  4. customThe crude product was recrystallized from a mixture of ethanol, ethyl acetate and water