反应详情

温度

80 °C

50 mg (0.158 mmol) of (E)-5-(3,4-dichlorostyryl)-2,3-dihydro-1H-benzo-1,4-diazepine were dissolved in a mixture of 0.1 ml of acetic anhydride and 1 ml of pyridine by heating to 80° C. The mixture was left to cool for 30 minutes then evaporated to dryness and the residue dissolved in water and ethyl acetate. The organic phase was dried over magnesium sulphate, filtered, evaporated to dryness and the residue chromatographed on silica gel using ethyl acetate for the elution. The product was dissolved in a solution of hydrogen chloride in ethyl acetate, evaporated to dryness and the residue dissolved in a small volume of acetone and left to crystallize. There was obtained 12 mg of (E)-1-acetyl-5-(3,4-dichlorostyryl)-2,3-dihydro-1H-1,4-benzodiazepine hydrochloride as an off-white solid. MS: m/e 358.9 [M+H]+.

1. waitThe mixture was left
2. temperatureto cool for 30 minutes
3. customthen evaporated to dryness
4. dissolutionthe residue dissolved in water
5. dry with materialThe organic phase was dried over magnesium sulphate
6. filtrationfiltered
7. customevaporated to dryness
8. customthe residue chromatographed on silica gel
9. washfor the elution
10. dissolutionThe product was dissolved in a solution of hydrogen chloride in ethyl acetate
11. customevaporated to dryness
12. dissolutionthe residue dissolved in a small volume of acetone
13. waitleft
14. customto crystallize