反应详情

To a solution of amine 2-1 (620 mg) and pyridine (0.48 mL) in dichloromethane (10 mL) at 0° C. was added a solution of phosgene in toluene (1.72 mL, 1.9 M) and the mixture was stirred at the temperature for 1 h. The mixture was diluted with dichloromethane and washed with 1 N HCl and brine, and dried over Na2SO4. Filtration and concentration of the filtrate gave the crude product which was purified by chromatography. Eluting with 60% ethyl acetate in hexanes afforded the desired product 2-2 (560 mg). 1H NMR (400 MHz, acetone-d6): δ 4.61 (dd, 1H), 4.52 (t, 1H), 4.35 (dd, 1H), 3.80 (s, 3H), 3.48 (m, 1H), 3.15 (m, 1H), 2.47 (t, 2H), 1.75–1.35 (m, 8H).

1. washwashed with 1 N HCl and brine
2. dry with materialdried over Na2SO4
3. filtrationFiltration and concentration of the filtrate
4. customgave the crude product which
5. customwas purified by chromatography
6. washEluting with 60% ethyl acetate in hexanes