4-(chloromethyl)-1,3-dioxane

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: 7.7 Grams of 1-chloro-2,4-methylenedioxybutane and 6.4 g of cyclohexylmethylamine are dissolved in 80 ml of dimethylformamide (DMF). Thereto are added 9.4 g of potassium carbonate and 17.0 g of sodiumiodide. The mixture is refluxed for 3 hours with heating. DMF is removed by evaporation under reduced pressure. The residue is extracted with diethyl ether. The extract is washed with water and dried with anhdyrous magnesium sulfate. The solvent is removed by evaporation. The residue is purified by a silica gel column chromatography (chloroform:methanol=20:1) and then subjected to distillation by glass tube oven to obtain 4.5 of N-(2,4-methylenedioxy-1-butyl)-N-cyclohexylmethylamine. The mixture is refluxed for 3 hours with heating DMF is removed by evaporation under reduced pressure The residue is extracted with diethyl ether The extract is washed with water dried with anhdyrous magnesium sulfate The solvent is removed by evaporation The residue is purified by a silica gel column chromatography (chloroform:methanol=20:1) subjected to distillation by glass tube oven

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

実験手順: 7.7 Grams of 1-chloro-2,4-methylenedioxybutane and 6.4 g of cyclohexylmethylamine are dissolved in 80 ml of dimethylformamide (DMF). Thereto are added 9.4 g of potassium carbonate and 17.0 g of sodiumiodide. The mixture is refluxed for 3 hours with heating. DMF is removed by evaporation under reduced pressure. The residue is extracted with diethyl ether. The extract is washed with water and dried with anhdyrous magnesium sulfate. The solvent is removed by evaporation. The residue is purified by a silica gel column chromatography (chloroform: methanol=20:1) and then subjected to distillation by glass tube oven to obtain 4.5 of N-(2,4-methylenedioxy-1-butyl)-N-cyclohexylmethylamine. The mixture is refluxed for 3 hours with heating DMF is removed by evaporation under reduced pressure The residue is extracted with diethyl ether The extract is washed with water dried with anhdyrous magnesium sulfate The solvent is removed by evaporation The residue is purified by a silica gel column chromatography (chloroform: methanol=20:1) subjected to distillation by glass tube oven

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

実験手順: 7.7 Grams of 1-chloro-2,4-methylenedioxybutane and 6.4 g of cyclohexylmethylamine are dissolved in 80 ml of dimethylformamide (DMF). Thereto are added 9.4 g of potassium carbonate and 17.0 g of sodiumiodide. The mixture is refluxed for 3 hours with heating. DMF is removed by evaporation under reduced pressure. The residue is extracted with diethyl ether. The extract is washed with water and dried with anhdyrous magnesium sulfate. The solvent is removed by evaporation. The residue is purified by a silica gel column chromatography (chloroform:methanol=20:1) and then subjected to distillation by glass tube oven to obtain 4.5 of N-(2,4-methylenedioxy-1-butyl)-N-cyclohexylmethylamine. The mixture is refluxed for 3 hours with heating DMF is removed by evaporation under reduced pressure The residue is extracted with diethyl ether The extract is washed with water dried with anhdyrous magnesium sulfate The solvent is removed by evaporation The residue is purified by a silica gel column chromatography (chloroform:methanol=20:1) subjected to distillation by glass tube oven