反应详情

To a suspension of (3RS)-1-(benzothiazol-2-yl)methyl-2,3-dihydro-5-(2-fluorophenyl)-3-phthalimido-1H-1,4-benzodiazepin-2-one (1.30 g) in THF (50 ml) was added dropwise hydrazine monohydrate (0.12 g) under stirring at ambient temperature. The mixture was stirred for 2 hours at the same temperature and refluxed under stirring for 2 hours. The reaction mixture was cooled in an ice-bath. The resultant precipitates were filtered off atad washed with THF (30 ml). The filtrate and washing were combined and concentrated in vacuo to afford a crude product. The product was dissolved into ethyl acetate (150 ml) and extracted with 1N-HCl aqueous solution (3×25 ml). The aqueous layer was alkalined with sodium bicarbonate and extracted with ethyl acetate (2×100 ml). The extracts were dried over magnesium sulfate and filtered off by filtration. The filtrate was concentrated in vacuo to afford (3RS)-3-amino-1-(benzo-thiazol-2-yl)methyl-2,3-dihydro-5-(2-fluorophenyl)-1H-1,4-benzo-diazepin-2-one as a colorless crystalline solid (110 mg). The compound was allowed to use in a next reaction step without further purification.

1. stirringThe mixture was stirred for 2 hours at the same temperature
2. temperaturerefluxed
3. stirringunder stirring for 2 hours
4. temperatureThe reaction mixture was cooled in an ice-bath
5. customThe resultant precipitates
6. filtrationwere filtered off
7. washatad washed with THF (30 ml)
8. washThe filtrate and washing
9. concentrationconcentrated in vacuo
10. customto afford a crude product
11. extractionextracted with 1N-HCl aqueous solution (3×25 ml)
12. extractionextracted with ethyl acetate (2×100 ml)
13. dry with materialThe extracts were dried over magnesium sulfate
14. filtrationfiltered off by filtration
15. concentrationThe filtrate was concentrated in vacuo