Triethylsilane → 2-propylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one
Reaktionsgleichung
[C:1]([C:5]1[S:19][C:8]2[O:9][C:10]3[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=3[NH:12][C:13](=[O:14])[C:7]=2[CH:6]=1)(=O)[CH2:2][CH3:3].C([SiH](CC)CC)C>>[CH2:1]([C:5]1[S:19][C:8]2[O:9][C:10]3[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=3[NH:12][C:13](=[O:14])[C:7]=2[CH:6]=1)[CH2:2][CH3:3]Komponenten
3
Versuchsvorschrift
2-Propionylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.2 g) was dissolved in trifuoroacetic acid (20 ml) and triethylsilane (2 g) was added. The mixture was stirred at room temperature for 20 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-propylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (930 mg).
Aufarbeitung
- additionwas added
- 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
Quellen und Nachweise
- ORD-Eintrag
- ord-a4db94400f894aad879fe15e4a33e021
- Quelldatensatz
- uspto-grants-2001_08
- Patentnummer
- US06271225B1
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