HRID26703

反应详情

EQUATION

反应方程式

HRID 26703 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 0.9 g of sodium hydroxide in 50 ml of water was added to a suspension of 1.66 g of ethyl 5-methyl-4,5-dihydro-4-oxo-pyrrolo[1,2-a]quinoxaline-2-carboxylate in 30 ml of hot ethanol and the mixture was warmed on a water bath for one hour after which thin layer chromatography showed no ester present. The resulting solution was filtered hot and the filtrate was acidified to a pH of 1-2 with concentrated hydrochloric acid. The mixture was cooled and filtered and the recovered product was rinsed with water and dried over P2O5 under vacuum to obtain 1.40 g (95% yield) of 5-methyl-4,5-dihydro-4-oxo-pyrrolo[1,2-a]quinoxaline-2-carboxylic acid melting at 330°-333° C.

WORKUP

后处理

  1. temperaturethe mixture was warmed on a water bath for one hour after which thin layer chromatography
  2. filtrationThe resulting solution was filtered hot
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. washthe recovered product was rinsed with water
  6. dry with materialdried over P2O5 under vacuum