反应详情

To a stirred solution of methyl (2RS,5SR)-5-(4-fluoro-phenyl)-pyrrolidine-2-carboxylate (2.27 g, 10.2 mmol) and triethylamine (2.13 ml, 15.3 mmol) in dichloromethane (60 ml) was added at 0° C. toluene-4-sulfonyl chloride (2.32 g, 12.2 mmol). The mixture was stirred at RT for 16 h, evaporated, dissolved in water (50 ml) and extracted with dichloromethane (2×40 ml). The combined organic layers were washed with water (40 ml), brine (40 ml), dried (MgSO4) and evaporated. The crude product was purified by crystallization from diethyl ether/hexane to give the title compound, off-white solid, m.p. 91° C. and MS: m/e=378.3 (M+H+).

1. customevaporated
2. dissolutiondissolved in water (50 ml)
3. extractionextracted with dichloromethane (2×40 ml)
4. washThe combined organic layers were washed with water (40 ml), brine (40 ml)
5. dry with materialdried (MgSO4)
6. customevaporated
7. customThe crude product was purified by crystallization from diethyl ether/hexane