反应详情

2-Hydroxymethylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.0 g) was dissolved in methylene chloride (10 ml) and triethylamine (450 mg) and methanesulfonyl chloride (500 mg) were added. The mixture was stirred at room temperature for 15 minutes and the solvent was evaporated under reduced pressure. Thereto was added 2M dimethylamine/methanol and the mixture was stirred at room temperature for 14 hours. The solvent was evaporated under reduced pressure and chloroform was added to the residue. After washing with water, the aqueous layer was extracted twice with chloroform. The organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) to give 2-(N,N-dimethylaminomethyl)thieno[2,3-b][1,5]benzoxazepin-4(5H)-one (500 mg).

1. customthe solvent was evaporated under reduced pressure
2. additionThereto was added 2M dimethylamine/methanol
3. stirringthe mixture was stirred at room temperature for 14 hours
4. customThe solvent was evaporated under reduced pressure and chloroform
5. additionwas added to the residue
6. washAfter washing with water
7. extractionthe aqueous layer was extracted twice with chloroform
8. dry with materialThe organic layer was dried over sodium sulfate
9. customthe solvent was evaporated under reduced pressure
10. customThe residue was purified by silica gel column chromatography (ethyl acetate)