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 NaHCO and brine. The organic layer is dried with Na2 SO4 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 NaHCO and brine
6. customThe organic layer is dried with Na2 SO4
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