3-(dimethylamino)-2H-furan-5-one

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 3.9 g of potassium hydrogen sulphate are added at room temperature to a suspension of 4.1 g of 4-(dimethylamino)furan-2(5H)-one and 5 g of N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethylamine in 50 ml of butyronitrile. The mixture is refluxed for 8 h. Thereafter, cooling at room temperature and washing twice with 50 ml of water are effected. The solvent is removed in vacuo. 6 g of 4-[[(6-chloropyridin-3-yl)methyl](2,2-difluoroethyl)amino]furan-2(5H)-one are obtained with a purity of 92% (82% yield). The mixture is refluxed for 8 h washing twice with 50 ml of water The solvent is removed in vacuo

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2 g (0.18 mol) of 4-(methylamino)furan-2(5H)-one are introduced in 20 ml of 1,2-dimethoxyethane, and 0.72 g of sodium hydroxide is added. 2.2 g of dimethyl sulphate in 5 ml of 1,2-dimethoxyethane are metered into the suspension and stirred at 40° C. for 5 h. The solvent is removed in vacuo and 50 ml of water are added to the residue. This mixture is then extracted with 50 ml of dichloromethane. The organic phase is dried over sodium sulphate and then evaporated down in vacuo. 1.2 g of 4-(dimethylamino)furan-2(5H)-one are obtained as a solid with a purity of 96% (yield 51%). The solvent is removed in vacuo and 50 ml of water are added to the residue This mixture is then extracted with 50 ml of dichloromethane The organic phase is dried over sodium sulphate evaporated down in vacuo