HRID133131

反应详情

EQUATION

反应方程式

HRID 133131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of tert-butyl (3R,6S)-6-(2,3-difluorophenyl)-2-oxo-1-(2,2,2-trifluoroethyl)azepan-3-ylcarbamate from Step F (135 mg, 0.320 mmol) in CH2Cl2 (5 mL) was added CF3CO2H (2.5 mL). After 30 min, the solution was concentrated in vacuo and azeotroped with toluene (2×). Saturated aqueous NaHCO3 was added and the mixture was extracted with CH2Cl2 (3×). The combined organic extracts were washed with brine, dried over MgSO4, filtered and concentrated in vacuo to give the title compound. MS: m/z=323 (M+1).

WORKUP

后处理

  1. concentrationthe solution was concentrated in vacuo
  2. customazeotroped with toluene (2×)
  3. additionSaturated aqueous NaHCO3 was added
  4. extractionthe mixture was extracted with CH2Cl2 (3×)
  5. washThe combined organic extracts were washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo