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 (0.037 g, 0.112 mmol) and 4-nitrophenylchloroformate (0.0238 g, 0.112 mmol) in dry tetrahydrofuran (2 mL) was cooled to 0° C. under argon. Triethylamine (0.011 g, 0.112 mmol) was added and the reaction stirred for 1 h. 3-Piperidin-4-yl-3,4-dihydropyrido[2,3-d]pyrimidin-2(1H)-one bisTFA salt (0.112 mmol) in DMSO (1 mL) followed by triethylamine (0.055 g) in were added. The reaction was allowed to come to room temperature and stirred for 4 h. The reaction was concentrated and purified by reverse phase HPLC (C-18, 5% to 95% 0.1% trifluoroacetic acid/acetonitrile in 0.1% aqueous trifluoroacetic acid gradient elution) to give TFA salt of the title compound (0.023 g, 29% yield). MS 592.2261 (M+1).

1. additionin were added
2. customto come to room temperature
3. stirringstirred for 4 h
4. concentrationThe reaction was concentrated
5. custompurified by reverse phase HPLC (C-18, 5% to 95% 0.1% trifluoroacetic acid/acetonitrile in 0.1% aqueous trifluoroacetic acid gradient elution)