反应详情

A solution of 70 g of [(2-amino-thiophen-3-yl)-(2-fluoro-phenyl)-methyleneamino]acetonitrile in 980 ml of acetic acid was stirred at 65° C. under argon for 1.5 h. After cooling the solvent was removed in a vacuum, the residue was dissolved in dichloromethane and neutralized with sodium bicarbonate solution while cooling with ice and extracted. The dichloromethane extracts were dried with sodium sulphate, filtered and evaporated to dryness in a vacuum. After crystallization from dichloromethane there were obtained 17.1 g of 5-(2-fluoro-phenyl)-3H-thieno[2,3-e][1,4]diazepin-2-ylamine of m.p. 219-220° C. (dec.).

1. temperatureAfter cooling the solvent
2. customwas removed in a vacuum
3. dissolutionthe residue was dissolved in dichloromethane and neutralized with sodium bicarbonate solution
4. temperaturewhile cooling with ice
5. extractionextracted
6. dry with materialThe dichloromethane extracts were dried with sodium sulphate
7. filtrationfiltered
8. customevaporated to dryness in a vacuum
9. customAfter crystallization from dichloromethane