HRID2363753

反应详情

EQUATION

反应方程式

HRID 2363753 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 500 mg of ethyl 6-[(trimethylsilyl)ethynyl]imidazo[1,2-a]pyridine-2-carboxylate in 10 mL of anhydrous tetrahydrofuran, cooled to 0° C. are added dropwise 1.58 mL of a 1M solution of tetrabutylammonium fluoride in tetrahydrofuran. The reaction mixture is stirred for 30 minutes, 5 mL of water are then added and the resulting mixture is extracted three times with 20 mL of dichloromethane. The product is purified by chromatography on silica, eluting with mixtures of ethyl acetate and hexane (from 1/3 to 1/1). The fractions containing the expected product are combined and concentrated to dryness under reduced pressure to give 280 mg of ethyl 6-ethynylimidazo[1,2-a]pyridine-2-carboxylate in the form of a yellow solid.

WORKUP

后处理

  1. extractionthe resulting mixture is extracted three times with 20 mL of dichloromethane
  2. customThe product is purified by chromatography on silica
  3. washeluting with mixtures of ethyl acetate and hexane (from 1/3 to 1/1)
  4. additionThe fractions containing the expected product
  5. concentrationconcentrated to dryness under reduced pressure