HRID37467

反应详情

EQUATION

反应方程式

HRID 37467 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

In 13 ml of acetic anhydride was suspended 5.0 g of 3,4-diethoxycarbonyl-6-phenyl-2-pyridone; and the suspension was cooled to -10° C. Fuming nitric acid (1.32 ml; 2.0 eq.) was added dropwise over 1 hour, and the mixture was stirred for 45 minutes as it is. After 40 ml of water was added, the mixture was stirred at room temperature and left standing overnight. The resulting crystals were collected by filtration and dried. Yield: 4.61 g (80.7%). The crystals were recrystallized from ethanol, to give pale yellow needles.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature
  2. waitleft
  3. waitstanding overnight
  4. filtrationThe resulting crystals were collected by filtration
  5. customdried
  6. customThe crystals were recrystallized from ethanol
  7. customto give pale yellow needles