HRID1437155

反应详情

EQUATION

反应方程式

HRID 1437155 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.0 g (3.66 mmol) of 4-(1H-pyrrolo[2,3-b]pyridin-3-yl)piperidine-1-carboxylic acid ethyl ester were dissolved in 10 ml of DMF and, at room temperature, 0.19 g (4.76 mmol) of 60% sodium hydride were carefully added. This mixture was stirred for half an hour. 0.45 ml (5.12 mmol) of 1-bromo-2-methoxyethane were added dropwise and the mixture was further stirred for 24 hours at 60° C. The reaction mixture was cooled to room temperature and poured over cold water. The aqueous phase was extracted twice with dichloromethane and the organic phase was washed with water and brine, dried with magnesium sulphate, filtered and evaporated to dryness. This resulted in 0.86 g (71% of yield) of product.

WORKUP

后处理

  1. stirringthe mixture was further stirred for 24 hours at 60° C
  2. extractionThe aqueous phase was extracted twice with dichloromethane
  3. washthe organic phase was washed with water and brine
  4. dry with materialdried with magnesium sulphate
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customThis resulted in 0.86 g (71% of yield) of product