HRID1739674

反应详情

EQUATION

反应方程式

HRID 1739674 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

A mixture of N,N-diethylglycine hydrochloride (96 mg, 0.57 mmol) and carbonyldiimidazole (92 mg, 0.57 mmol) in THF (5 mL) were refluxed under a nitrogen atmosphere for 15 min. With the bath temperature at 70° C., DMF (7 mL) and 6-nitro-pyridoquinoxalinedione (0.1 g, 0.38 mmol) were added, and finally triethylamine (265 μL) was added and the reaction heated for 14 h at 80° C. The solvent was removed and the residue triturated with water, collected by filtration and washed with diethyl ether. An orange brown solid (104 mg) was obtained in 73% yield, mp 285-290° C. (dec); m/e M+1 376, nmR, IR.

WORKUP

后处理

  1. temperaturewere refluxed under a nitrogen atmosphere for 15 min
  2. customThe solvent was removed
  3. customthe residue triturated with water
  4. filtrationcollected by filtration
  5. washwashed with diethyl ether