4-(甲氨基)呋喃-2(5H)-酮

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 30 g of 4-(methylamino)furan-2(5H)-one (Example 11) are initially charged in 450 ml of dimethoxyethane at room temperature. Subsequently, 12.6 g of sodium hydroxide are added and, at 40° C., 225 g of a 20% solution of 2-chloro-5-(chloromethyl)pyridine in dimethoxyethane are metered in. The mixture is stirred at 50° C. for a further 6 h. The solvent is substantially removed under reduced pressure and the residue is admixed with 300 ml of water. The solids are filtered off, washed with 150 ml of water and dried under reduced pressure. 58.7 g of 4-([[6-chloropyridin-3-yl]methyl](methy)amino)furan-2(5H)-one are obtained with a purity of 94% (this corresponds to 87% yield). The solvent is substantially removed under reduced pressure The solids are filtered off washed with 150 ml of water dried under reduced pressure

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 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

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 30 g of 4-(methylamino)furan-2(5H)-one (Example 11) are initially charged in 450 ml of dimethoxyethane at room temperature. Subsequently, 12.6 g of sodium hydroxide are added and, at 40° C., 225 g of a 20% solution of 2-chloro-5-(chloromethyl)pyridine in dimethoxyethane are metered in. The mixture is stirred at 50° C. for a further 6 h. The solvent is substantially removed under reduced pressure and the residue is admixed with 300 ml of water. The solids are filtered off, washed with 150 ml of water and dried under reduced pressure. 58.7 g of 4-([[6-chloropyridin-3-yl]methyl](methy)amino)furan-2(5H)-one are obtained with a purity of 94% (this corresponds to 87% yield). The solvent is substantially removed under reduced pressure The solids are filtered off washed with 150 ml of water dried under reduced pressure