反应详情

A solution of 1.2 g of ethyl 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-7-carboxylate in 100 ml of methylene chloride is cooled to 0° C. and 10 ml of triethylamine added followed by 1.5 g of 4-[(2-methylbenzoyl)amino)benzoyl chloride. The reaction mixture is stirred at room temperature for 18 hours and concentrated in vacuo to a residue which is partitioned between water and chloroform. The organic layer is dried over Na2SO4 and concentrated in vacuo to a residue. The residue is purified by column chromatography on silica gel by elution with 40% ethyl acetate-hexane to give 1.0 g of the desired product as a solid; mass spectrum (M+H)494.

1. concentrationconcentrated in vacuo to a residue which
2. customis partitioned between water and chloroform
3. dry with materialThe organic layer is dried over Na2SO4
4. concentrationconcentrated in vacuo to a residue
5. customThe residue is purified by column chromatography on silica gel by elution with 40% ethyl acetate-hexane