反应详情

16.7 g (0.0453 mol) of the product obtained in step b) were dissolved in 150 ml of absolute dioxane, and the resulting solution was admixed with 6.7 g (0.14 mol) of a 50% dispersion of sodium hydride in mineral oil. Thereafter, the mixture--while protected against the external atmosphere by a low flow of nitrogen--was refluxed until no starting material could be detected by TLC. The surplus of sodium hydride was decomposed by cautious addition of 10 ml of a mixture of methanol and tetrahydrofuran (50/50 v/v). The reaction mixture was neutralized by addition of acetic acid and then was evaporated in vacuo. The residue was purified by column chromatography on silica gel (0.2-0.5 mm) using successively dichloromethane/ethyl acetate 10/1 (v/v) and dichloromethane/ethyl acetate 1/1 (v/v) as eluents. The crystalline product obtained by evaporation of suitable fractions was recrystallized from acetonitrile and 2-propanol. The product had a m.p. of 213°-215° C. and was identified as 5,11-dihydro- 11-[(4-methoxyphenyl)-methyl]-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one. The yield was 10.3 g (68% of theory).

1. temperaturewas refluxed until no starting material
2. customwas evaporated in vacuo
3. customThe residue was purified by column chromatography on silica gel (0.2-0.5 mm)
4. customThe crystalline product obtained by evaporation of suitable fractions
5. customwas recrystallized from acetonitrile and 2-propanol