HRID2294205

反应详情

EQUATION

反应方程式

HRID 2294205 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

4 ml of trimethylsilylhydroxylamine (30 mmol) were sprayed at room temperature into a suspension of 1.38 g of ethyl 4-hydroxy-7-nitro-2-oxo-1,2-dihydro-quinoline-3 -carboxylate (5 mmol) in 40 ml of dioxan. After heating to 100° C. all passed slowly into solution. The reaction mixture was left to stir at 90° C. for 20 hrs., cooled to room temperature and the separated voluminous precipitate was filtered off. This was washed with water and dried in a high vacuum. 740 mg of 4,N-dihydroxy-7-nitro-2-oxo-1,2-dihydro-quinoline-3-carboxamide (65%) were obtained as pale beige crystals.

WORKUP

后处理

  1. waitThe reaction mixture was left
  2. temperature, cooled to room temperature
  3. filtrationthe separated voluminous precipitate was filtered off
  4. washThis was washed with water
  5. customdried in a high vacuum