反应详情

A mixture of the product from the previous reaction (2.80 g), potassium carbonate (10.0 g) and 1-[(2-methoxyphenyl)piperid-4-yl]methylamine (1.88 g) in dry acetonitrile (100 ml) was heated under reflux with stirring for 90 hours. The cooled mixture was filtered and the filtrate evaporated under reduced pressure to leave a pale-yellow oil. Purification by flash column chromatography on silica eluting with a 19:1 mixture of dichloromethane and methanol gave a pale-yellow oil which was then dissolved in ethanol (5 ml) and treated with a solution of fumaric acid (0.70 g) in ethanol (5 ml). The solvent was evaporated from the resulting solution under reduced pressure to give (S)-N-(2,3-dihydrofuro[3,2-f]-1,4-benzodioxin-2-ylmethyl)-1-[1-(2-methoxyphenyl)piperid-4-yl]methylamine monofumarate monohydrate (3.06 g) as a pale-yellow solid m.p. 95-6° C., [α]D=−38.5° (C=0.301, MeOH)

1. additionA mixture of the product
2. temperaturewas heated
3. temperatureunder reflux
4. filtrationThe cooled mixture was filtered
5. customthe filtrate evaporated under reduced pressure
6. customto leave a pale-yellow oil
7. customPurification by flash column chromatography on silica eluting
8. additionwith a 19:1 mixture of dichloromethane and methanol
9. customgave a pale-yellow oil which
10. customThe solvent was evaporated from the resulting solution under reduced pressure