反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
2-Acetylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.5 g) was dissolved in trifluoroacetic acid (20 ml) and triethylsilane (2 g) was added. The mixture was stirred at room temperature for 42 hours. The solvent was evaporated under reduced pressure and the residue was dissolved in chloroform. The mixture was washed with water and saturated aqueous sodium hydrogencarbonate solution, and dried over sodium sulfate. The solvent was evaporated under reduced pressure. To the residue were added chloroform and ethyl acetate and the precipitated crystals were collected by filtration. The obtained crystals were washed with diisopropyl ether to give 2-ethylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.1 g).
WORKUP
后处理
- customThe solvent was evaporated under reduced pressure
- dissolutionthe residue was dissolved in chloroform
- washThe mixture was washed with water and saturated aqueous sodium hydrogencarbonate solution
- dry with materialdried over sodium sulfate
- customThe solvent was evaporated under reduced pressure
- additionTo the residue were added chloroform and ethyl acetate
- filtrationthe precipitated crystals were collected by filtration
- washThe obtained crystals were washed with diisopropyl ether