HRID523452

反应详情

EQUATION

反应方程式

HRID 523452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

286 mg (1.49 mmol) of 4-methyl-2-(pyridin-3-yl)-1,3-thiazole-5-amine were dissolved in THF, 0.52 ml of triethylamine was added, and 263 mg of trifluoropropionyl chloride were added while cooling with an ice bath. The mixture was stirred at room temperature overnight and then concentrated. Ethyl acetate, saturated sodium chloride solution and aqueous phosphate buffer pH=7 were added to the residue, the aqueous phase was extracted twice with ethyl acetate, and the combined organic phases were dried over Na2SO4 and concentrated. The residue was purified by chromatography (silica gel, cyclohexane, acetone).

WORKUP

后处理

  1. temperaturewhile cooling with an ice bath
  2. concentrationconcentrated
  3. additionEthyl acetate, saturated sodium chloride solution and aqueous phosphate buffer pH=7 were added to the residue
  4. extractionthe aqueous phase was extracted twice with ethyl acetate
  5. dry with materialthe combined organic phases were dried over Na2SO4
  6. concentrationconcentrated
  7. customThe residue was purified by chromatography (silica gel, cyclohexane, acetone)