HRID1066857

反应详情

EQUATION

反应方程式

HRID 1066857 的结构方程式

PROCEDURE

实验过程

Under an argon atmosphere 4-methyl-1H-indole-2-carboxylic acid (0.64 g, 3.65 mmol) was dissolved in 20 ml of methanol. Concentrated sulfuric acid (0.5 ml) was added and the resulting mixture was heated to reflux and maintained at this temperature overnight. The progress of the reaction was monitored by thin layer chromatography. Some solvent was removed in vacuo and the resulting crystals were removed by filtration. The solids were taken up in diethyl ether, washed twice with saturated sodium bicarbonate, and then once with brine. The organic fraction was dried over magnesium sulfate and the solvents were removed in vacuo.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureto reflux
  3. temperaturemaintained at this temperature overnight
  4. customSome solvent was removed in vacuo
  5. customthe resulting crystals were removed by filtration
  6. washwashed twice with saturated sodium bicarbonate
  7. dry with materialThe organic fraction was dried over magnesium sulfate
  8. customthe solvents were removed in vacuo