HRID337971

反应详情

EQUATION

反应方程式

HRID 337971 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of the 5-[(1R*,2S*)-2-(benzyloxy)cyclopentyl]-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole (1.15 g, 3.52 mmol) prepared in Example 148a in dichloromethane (10 mL), trifluoroacetic acid (5.0 mL) was added at room temperature, and the reaction solution was stirred for 12 hours. The reaction solution was concentrated, and a saturated aqueous solution of sodium hydrogencarbonate (50 mL) was added to the residue, followed by extraction with ethyl acetate (50 mL). The thus obtained organic layer was washed with saturated saline (50 mL) and dried over anhydrous sodium sulfate. After vacuum concentration, the residue was purified with silica gel chromatography (hexane/ethyl acetate=1:1) to yield the title compound (840 mg, 98%) as a pale yellow oil.

WORKUP

后处理

  1. concentrationThe reaction solution was concentrated
  2. additiona saturated aqueous solution of sodium hydrogencarbonate (50 mL) was added to the residue
  3. extractionfollowed by extraction with ethyl acetate (50 mL)
  4. washThe thus obtained organic layer was washed with saturated saline (50 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationAfter vacuum concentration
  7. customthe residue was purified with silica gel chromatography (hexane/ethyl acetate=1:1)