HRID489614

反应详情

EQUATION

反应方程式

HRID 489614 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-ethyl-1H-indole-3-carboxylic acid methyl ester (1.8 g, 8.8 mmol) was stirred in a 1:1 mixture of THF:MeOH (40 mL), and to this was added 2N NaOH (20 mL). The reaction was heated at reflux for 4 hours. The reaction mixture was partially evaporated to remove the THF, MeOH and the remaining material diluted with water (20 mL) and acidified to pH=2 with 1N HCl. The mixture was extracted with dichloromethane (100 mL), dried over sodium sulfate and evaporated under reduced pressure to give the title compound as a white solid, which was used directly in the next step.

WORKUP

后处理

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 4 hours
  3. customThe reaction mixture was partially evaporated
  4. customto remove the THF, MeOH
  5. additionthe remaining material diluted with water (20 mL)
  6. extractionThe mixture was extracted with dichloromethane (100 mL)
  7. dry with materialdried over sodium sulfate
  8. customevaporated under reduced pressure