反应详情

温度

25 °C

To a mixture of 4-amino-piperidine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl ester (1.3 g, 5 mmol] and 4-(2-methyl-quinolin-4-ylmethoxy)-benzenesulfonyl chloride hydrochloride (1.9 g, 5.50 mmol) in CH2Cl2 (20 mL) was added saturated aqueous NaHCO3 (20 mL) at 0° C. The solution was allowed to warm to 25° C. over 19 h. The reaction was then further diluted in CH2Cl2 (100 mL) and water (30 mL). The organic layer was washed with water (2×50 mL). The organic layer was dried over MgSO4, filtered and concentrated to provide a crude oil (2.6 g). The crude product was purified by Biotage Flash 40M chromatography, eluting with 1:1 ethyl acetate-hexanes, to afford 4-[4-(2-methyl-quinolin-4-ylmethoxy)-benzenesulfonylamino]-piperidine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl ester as a white solid (1.6 g, 55%). MS: 570 (M+H)+

1. washThe organic layer was washed with water (2×50 mL)
2. dry with materialThe organic layer was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. customto provide a crude oil (2.6 g)
6. customThe crude product was purified by Biotage Flash 40M chromatography
7. washeluting with 1:1 ethyl acetate-hexanes