反应详情

温度

0 °C

To a suspension of Methyl[(3S)-5-(4-chlorophenyl)-7-(methyloxy)-2-thioxo-2,3-dihydro-1H-1,4-benzodiazepin-3-yl]acetate (for a preparation see Reference compound E (9.0 g, 23.2 mmol) in THF (300 mL) at 0° C. was added hydrazine monohydrate (3.4 mL, 69.6 mmol) dropwise. The reaction mixture was stirred for 5 h between 5° C. and 15° C. before being cooled at 0° C. Et3N (9.7 mL, 69.6 mmol) was then added slowly and acetyl chloride (7.95 mL, 69.6 mmol) was added dropwise. The mixture was then allowed to warm to room temperature for 16 h before being concentrated under reduced pressure. The crude product was dissolved in DCM and washed with water. The organic layer was dried over Na2SO4, filtered and concentrated in vacuo to give the crude title compound (9.7 g, 98% yield) which was used without further purification. Rf=0.49 (DCM/MeOH: 90/10).

1. customat 0° C.
2. temperatureto warm to room temperature for 16 h
3. concentrationbefore being concentrated under reduced pressure
4. dissolutionThe crude product was dissolved in DCM
5. washwashed with water
6. dry with materialThe organic layer was dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo