反应详情

温度

2.5 °C

Methyl 2-(4-chlorophenyl)-1-phenyl-6,7-dihydro-5H-pyrrolizine-3-carboxylate (0.87 g, 2.5 mmol) is dissolved in dichloroethane (10 ml) and the solution is cooled to 0-5° C. in an ice bath. A solution of chlorosulphonic acid (0.5 g, 5.7 mmol) in dichloroethane (5 ml) is slowly added dropwise (IT<10° C.), and the mixture is then stirred at RT for 12 h. A solution of NH3 in dichloroethane saturated in the cold is added, and the mixture is stirred at RT for a further 12 h. The mixture is then treated with water (20 ml), and the organic phase is separated in a separating funnel. Solid which is insoluble in water is filtered off from the aqueous phase with suction and dried in vacuo. The dried solid substance is crystallized from MeOH: 0.5 g (47%); a 2nd crystal fraction crystallized from the mother liquor in the cold: 23% (0.25 g).

1. stirringthe mixture is stirred at RT for a further 12 h
2. customthe organic phase is separated in a separating funnel
3. filtrationis filtered off from the aqueous phase with suction
4. customdried in vacuo
5. customThe dried solid substance is crystallized from MeOH
6. customa 2nd crystal fraction crystallized from the mother liquor in the cold: 23% (0.25 g)