oxolan-2-ylmethyl methanesulfonate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1.42 g of (tetrahydro-2-furanyl)methyl methanesulfonate, 5 ml of ethylendiamine, 1.53 g of potassium carbonate, anhydrous, and 0.1 g of sodium iodide was stirred at 60° C. for 4 hours. After the completion of reaction, ethyl acetate was added, and insolubles were then removed by filtration. The filtrate was concentrated under a reduced pressure, and the resultant residue was poured into 10 ml of a 6N aqueous solution of sodium hydroxide, followed by extraction with 100 ml of methylene chloride. Next, the extract was dried over sodium sulfate, anhydrous, and then concentrated under a reduced pressure to obtain 1.2 g of N-[(tetrahydro-2-furanyl) methyl]ethylenediamine as a yellow oil. was added insolubles were then removed by filtration The filtrate was concentrated under a reduced pressure the resultant residue was poured into 10 ml of a 6N aqueous solution of sodium hydroxide followed by extraction with 100 ml of methylene chloride Next, the extract was dried over sodium sulfate, anhydrous concentrated under a reduced pressure

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1.42 g of (tetrahydro-2-furanyl)methyl methanesulfonate, 5 ml of ethylendiamine, 1.53 g of potassium carbonate, anhydrous, and 0.1 g of sodium iodide was stirred at 60° C. for 4 hours. After the completion of reaction, ethyl acetate was added, and insolubles were then removed by filtration. The filtrate was concentrated under a reduced pressure, and the resultant residue was poured into 10 ml of a 6N aqueous solution of sodium hydroxide, followed by extraction with 100 ml of methylene chloride. Next, the extract was dried over sodium sulfate, anhydrous, and then concentrated under a reduced pressure to obtain 1.2 g of N-[(tetrahydro-2-furanyl) methyl]ethylenediamine as a yellow oil. was added insolubles were then removed by filtration The filtrate was concentrated under a reduced pressure the resultant residue was poured into 10 ml of a 6N aqueous solution of sodium hydroxide followed by extraction with 100 ml of methylene chloride Next, the extract was dried over sodium sulfate, anhydrous concentrated under a reduced pressure

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

実験手順: Mesyl chloride (6.17 g) was dropwise added to a solution of 5.0 g of (tetrahydro-2furanyl)methanol, 2.18 g of triethylamine and 30 ml of tetrahydrofuran under ice-cooling over 30 minutes, followed by stirring at the same temperature for 2 hours. After the completion of reaction, the insolubles were filtered, and the filtrate was then concentrated under a reduced pressure to obtain (tetrahydro-2-furanyl)methyl methanesulfonate as an oil. cooling over 30 minutes After the completion of reaction the insolubles were filtered the filtrate was then concentrated under a reduced pressure

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

実験手順: A mixture of piperid-4-one oxime (46 g; 0.04 moles), 2-tetrahydrofurylmethyl methanesulphonate (79.3 g; 0.44 moles) and anhydrous potassium carbonate (56.5 g; 0.40 moles) in methyl isobutyl ketone (625 ml), was boiled under reflux with stirring for 48 hours. After cooling, the reaction mixture was washed with brine, dried (Na2SO4), and the solvent removed in vacuo. The residue was crystallised from diisopropyl ether to give 1-(2-tetrahydrofurylmethyl)-piperid-4-one oxime (42.5 g), m.p. 104°-106°. under reflux After cooling the reaction mixture was washed with brine dried (Na2SO4) the solvent removed in vacuo The residue was crystallised from diisopropyl ether