HRID68382

反应详情

EQUATION

反应方程式

HRID 68382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(3aR*,4R*,6aS*)-6a-(5-Bromo-2,4-difluorophenyl)-4-methylhexahydro furo[3,4-c]isoxazole (200 mg, 0.62 mmol) was dissolved in THF (10 mL). Zinc dust (0.49 g, 7.50 mmol) was added, followed by acetic acid (143 μl, 2.50 mmol) and the reaction was stirred at room temperature overnight. The reaction was filtered through Celite®, washing with MeOH and the filtrate was concentrated in vacuo. The residue was basified with saturated NaHCO3 and DCM added. The mixture was filtered and the layers separated. The aqueous layer was extracted with DCM (×2) and the combined organics were dried (MgSO4) and concentrated to leave the title compound (120 mg).

WORKUP

后处理

  1. filtrationThe reaction was filtered through Celite®
  2. washwashing with MeOH
  3. concentrationthe filtrate was concentrated in vacuo
  4. additionadded
  5. filtrationThe mixture was filtered
  6. customthe layers separated
  7. extractionThe aqueous layer was extracted with DCM (×2)
  8. dry with materialthe combined organics were dried (MgSO4)
  9. concentrationconcentrated