反应详情

温度

70 °C

A stirred suspension of 8-chloro-6-phenyl-1-[(phthalimidooxy)methyl]-4H-s-triazolo[4,3-a][1,4]benzodiazepine (9.4 g., 0.02 mole) in absolute ethanol (100 ml.) was treated with hydrazine hydrate (1.45 ml.) and warmed, under nitrogen, at a bath temperature at 70° C. for 3 hours. The mixture was cooled in an ice bath and filtered. The solid was washed with ethanol and methylene chloride. The combined filtrate was concentrated in vacuo; the residue was mixed with water and extracted with methylene chloride. The extract was washed with water, dried over anhydrous sodium sulfate and concentrated. The residue was dissolved in chloroform-ethyl-acetate and filtered through a small pad of silica gel. The filtrate was crystallized from methanol-ethylacetate to give 1-[(aminooxy)methyl]-8-chloro-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine in three crops: 1.95 g. of melting point 190°-191.5° C.; 0.89 g. of melting point 183°-186° C.; 0.285 g. of melting point 183°-186° C. The analytical sample had a melting point 191°-192° C.

1. temperatureThe mixture was cooled in an ice bath
2. filtrationfiltered
3. washThe solid was washed with ethanol and methylene chloride
4. concentrationThe combined filtrate was concentrated in vacuo
5. additionthe residue was mixed with water
6. extractionextracted with methylene chloride
7. washThe extract was washed with water
8. dry with materialdried over anhydrous sodium sulfate
9. concentrationconcentrated
10. dissolutionThe residue was dissolved in chloroform-ethyl-acetate
11. filtrationfiltered through a small pad of silica gel
12. customThe filtrate was crystallized from methanol-ethylacetate