HRID473907

反应详情

EQUATION

反应方程式

HRID 473907 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 1,1-dimethylethyl 7-[4-(1-{[(2-methylpropyl)oxy]carbonyl}-1H-imidazol-2-yl)phenyl]-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (0.30 g, 0.61 mmol) in dichloromethane (100 mL) was added trifluoroacetic acid (20 mL) and the reaction mixture was heated to reflux. After cooling to room temperature the solvent was evaporated. The residue was dissolved in ethyl acetate (250 mL). The organic layer was washed with saturated aqueous sodium bicarbonate (2×100 mL), brine, dried over anhydrous sodium sulfate then filtered and concentrated to give 2-methylpropyl 2-[4-(2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)phenyl]-1H-imidazole-1-carboxylate (0.22 g, 92%). MS (EI) for C23H25N3O3: 392 (MH+).

WORKUP

后处理

  1. temperaturethe reaction mixture was heated to reflux
  2. customwas evaporated
  3. dissolutionThe residue was dissolved in ethyl acetate (250 mL)
  4. washThe organic layer was washed with saturated aqueous sodium bicarbonate (2×100 mL), brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationthen filtered
  7. concentrationconcentrated