HRID1426355

反应详情

EQUATION

反应方程式

HRID 1426355 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of tert-butyl 4-{[6-(1,2-dihydroxyethyl)-2-(trifluoromethyl)pyrimidin-4-yl]oxy}piperidine-1-carboxylate (542 mg, 1.33 mmol) in THF (10. mL) and water (6.0 mL) was added acetic acid (20. μL, 0.35 mmol) and sodium periodate (854 mg, 3.99 mmol) at −5° C. After stirring for 30 minutes, the reaction mixture was diluted with ether and water. The aqueous layer was extracted with ethyl acetate once and the combined organic layers were washed with brine and dried over anhydrous Na2SO4. The organic solvent was removed in vacuo and the residue was purified with silica gel column to give the desired product as colorless oil. LCMS (M+H)+: 376.1.

WORKUP

后处理

  1. extractionThe aqueous layer was extracted with ethyl acetate once
  2. washthe combined organic layers were washed with brine
  3. dry with materialdried over anhydrous Na2SO4
  4. customThe organic solvent was removed in vacuo
  5. customthe residue was purified with silica gel column