反应详情

A mixture of 4-tert-butoxycarbonylaminomethyl-2-tert-butoxycarbonylmethoxyaniline (930 mg, 2.61 mmol), (S)-9-chloro-5-carboxymethyl-6,7-dihydro-1H, 5H-pyrido[1,2,3-de]quinoxaline-2,3-dione (807 mg, 2.74 mmol), Bop-Cl (770 mg, 2.99 mmol), and triethylamine (2 mL) in dichloromethane (20 mL) was stirred for 4 days at room temperature. The mixture was diluted with ethyl acetate (500 mL) and washed with 5% aqueous potassium hydrogen sulfate, water, phosphate buffer (pH 7.5), water, and brine, successively, dried over magnesium sulfate, and concentrated. The residual solid was recrystallized from acetone-ethyl acetate to give 1.04 g of the title compound. The mother liquid was concentrated and the residue was purified by silica gel column chromatography with 0.3% acetic acid/ethyl acetate to give additionally 360 mg of the title compound. A total amount of 1.40 g of the title compound was obtained (85%).

1. washwashed with 5% aqueous potassium hydrogen sulfate, water, phosphate buffer (pH 7.5), water, and brine
2. dry with materialsuccessively, dried over magnesium sulfate
3. concentrationconcentrated
4. customThe residual solid was recrystallized from acetone-ethyl acetate