HRID133133

反应详情

EQUATION

反应方程式

HRID 133133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Pyridinium dichromate (765 mg, 2.035 mmol) was added to a solution of crude tert-butyl [(2Z,3R,6S)-6-(2,3-difluorophenyl)-2-({2-hydroxy-2-[1-(trifluoromethyl)cyclopropyl]ethyl}imino)azepan-3-yl]carbamate from Step A (200 mg, 0.407 mmol) in acetonitrile (5 mL). After 70 h at ambient temperature, the mixture was filtered and concentrated. Saturated aqueous NaHCO3 was added and the mixture was extracted with CH2Cl2 (3×). The combined organic extracts were dried over MgSO4, filtered, and concentrated under reduced pressure to give the title compound. MS: m/z=472 (M+1).

WORKUP

后处理

  1. filtrationthe mixture was filtered
  2. concentrationconcentrated
  3. additionSaturated aqueous NaHCO3 was added
  4. extractionthe mixture was extracted with CH2Cl2 (3×)
  5. dry with materialThe combined organic extracts were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure