HRID1360173

反应详情

EQUATION

反应方程式

HRID 1360173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.48 g (1.2 mmol) of t-butyl 4-hydroxy-3-{[4-(trifluoromethyl)benzoyl]amino}piperidin-1-carboxylate (product of step 1) was dissolved in 10 mL of methylene chloride, and 5.24 g (1.9 mmol) of Dess-Martin periodinane was dropwise added thereto. After stirring for 5 hours, 50 mL of ethylacetoacetate was dropwise added thereto, and the resulting solution was washed with water. An organic layer dried over anhydrous magnesium sulfate. The reaction solution was filtered off and distilled off under reduced pressure, then the residue was purified by column chromatography to give 0.30 g (0.78 mmol) of the title compound in a total yield of 65%.

WORKUP

后处理

  1. washthe resulting solution was washed with water
  2. dry with materialAn organic layer dried over anhydrous magnesium sulfate
  3. filtrationThe reaction solution was filtered off
  4. distillationdistilled off under reduced pressure
  5. customthe residue was purified by column chromatography