HRID1437164

反应详情

EQUATION

反应方程式

HRID 1437164 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.1 g (3.18 mmol) of 4-[1-(2-ethoxyethyl)-1H-pyrrolo[2,3-b]pyridin-3-yl]-piperidine-1-carboxylic acid ethyl ester were added to a solution of 2.1 g (31.8 mmol) of potassium hydroxide in 30 ml of isopropanol. The mixture was refluxed for 20 hours. The solvent was distilled off and cold water was added. This solution was acidified with concentrated hydrochloric acid and then basified with 8 N aqueous sodium hydroxide solution. This aqueous solution was extracted twice with ethyl acetate. The organic phase was washed with water and brine, dried over magnesium sulphate, filtered and evaporated under reduced pressure affording 0.65 g (75% of yield) of 1-(2-ethoxyethyl)-3-piperidinyl-1H-pyrrolo[2,3-b]pyridine obtained as an oil.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 20 hours
  2. distillationThe solvent was distilled off
  3. additioncold water was added
  4. extractionThis aqueous solution was extracted twice with ethyl acetate
  5. washThe organic phase was washed with water and brine
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. customevaporated under reduced pressure