反应详情

A solution of (3R) 3-amino-2-oxo-5-phenyl-1-(2,2,2-trifluorethyl)-2,3-dihydro-1H-1,4-benzodiazepine (0.030 g, 0.090 mmol) and 4-nitrophenylchloroformate (0.018 g, 0.090 mmol) in dry tetrahydrofuran (2 mL) was cooled to 0° C. under argon. Triethylamine (0.013 mL, 0.090 mmol) was added and the reaction stirred for 1 h. Solid 3-piperidin-4-yl-3,4-dihydropyrido[4,3-d]pyrimidin-2(1H)-one bisTFA salt (0.90 mmol) followed by triethylamine (0.065 mL) were added. The reaction was allowed to come to room temperature and stirred for 1 h. The reaction was quenched with 1N NaOH and concentrated. The crude product was purified by chromatography (silica gel, 0 to 15% methanol in methylene chloride gradient elution) to give the title compound (0.013 g, 24% yield). MS 592.2286 (M+1).

1. additionwere added
2. customto come to room temperature
3. stirringstirred for 1 h
4. customThe reaction was quenched with 1N NaOH
5. concentrationconcentrated
6. customThe crude product was purified by chromatography (silica gel, 0 to 15% methanol in methylene chloride gradient elution)