反应详情

温度

0 °C

To a mixture of 1.37 g (5 mmol) of 4-[(2-methylbenzoyl)amino]benzoyl chloride in 10 ml of methylene chloride, cooled to 0° C. is added 7 mmol of triethylamine and 5 mmol of 6,7-dihydro-5H-pyrrolo-[1,2-a][1,5]benzodiazepine. The cooling bath is removed and the reaction mixture is allowed to stir at room temperature for 48 hours. The volatiles are removed in vacuo to give a residue. The residue is dissolved in 100 ml of ethyl acetate and washed with water, 2N citric acid, aqueous NaHCO3 and brine. The solution is dried with Na2SO4 and the solvent removed in vacuo to give a solid. The solid is triturated with ether-hexane to give the desired product, mass spectrum (CI):422(M+H).

1. customThe cooling bath is removed
2. customThe volatiles are removed in vacuo
3. customto give a residue
4. washwashed with water, 2N citric acid, aqueous NaHCO3 and brine
5. dry with materialThe solution is dried with Na2SO4
6. customthe solvent removed in vacuo
7. customto give a solid
8. customThe solid is triturated with ether-hexane