HRID1289436

反应详情

EQUATION

反应方程式

HRID 1289436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

406 mg of 9-trifluoromethyl-2,3-dioxo-1,2,3,5,6,7-hexahydro-pyrido[1,2,3-de]quinoxaline-5-phosphonic acid diethyl ester in 2 ml of glacial acetic acid is mixed with 0.05 ml of water, 0.025 ml of concentrated sulfuric acid, 178 mg of iodine and 70 mg of iodic acid and stirred for 15 hours at 80° C. bath temperature. After concentration by evaporation, it is mixed with water and the product is suctioned off. 60 mg of 8-iodo-9-trifluoromethyl-2,3-dioxo-1,2,3,5,6,7-hexahydro-pyrido[1,2,3-de]quinoxaline-5-phosphonic acid of melting point 307° C. (with decomposition) is obtained.

WORKUP

后处理

  1. concentrationAfter concentration
  2. customby evaporation, it
  3. additionis mixed with water