反应详情

To a solution of 414.5 mg of 2,5-dichlorobenzoyl chloride in 5 ml of methylene chloride is added 276 μl of triethylamine. After stirring at 0° C. for 3 minutes 400 mg of the 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine is added. The bath is removed and the reaction mixture stirred at room temperature for 3 hours. The volatiles are concentrated in vacuo to give a residue which is dissolved in ethyl acetate and washed with water, 2N citric acid, 1M NaHCO3 and brine. The organic layer is dried with Na2SO4 and concentrated in vacuo to a residue which is purified by thick layer chromatography by elution with 1:1 ethyl acetate-hexanes to give a residue. The residue is crystallized from ethyl acetate to give 220 mg of the desired product as white crystals, m.p. 218°-220° C.

1. additionis added
2. customThe bath is removed
3. concentrationThe volatiles are concentrated in vacuo
4. customto give a residue which
5. washwashed with water, 2N citric acid, 1M NaHCO3 and brine
6. dry with materialThe organic layer is dried with Na2SO4
7. concentrationconcentrated in vacuo to a residue which
8. customis purified by thick layer chromatography by elution with 1:1 ethyl acetate-hexanes
9. customto give a residue
10. customThe residue is crystallized from ethyl acetate