decyl methanesulfonate

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: 77.3 Grams of decyl methylsulfonate, 44.64 grams of 1-ethoxycarbonylpiperazine, 500 ml. of ethanol, and 39 grams of potassium carbonate are combined and refluxed for approximately 44 hours under a nitrogen atmosphere. After cooling to room temperature the residue is dissolved in a mixture of water and ethyl ether. The organic layer is separated, washed three times with portions of water and dried over anhydrous sodium sulfate. The solvents are removed under reduced pressure to give 1-ethoxycarbonyl-4-decylpiperazine. refluxed for approximately 44 hours under a nitrogen atmosphere The organic layer is separated washed three times with portions of water dried over anhydrous sodium sulfate The solvents are removed under reduced pressure

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

実験手順: 77.3 Grams of decyl methylsulfonate, 44.64 grams of 1-ethoxycarbonylpiperazine, 500 ml. of ethanol, and 39 grams of potassium carbonate are combined and refluxed for approximately 44 hours under a nitrogen atmosphere. After cooling to room temperature the residue is dissolved in a mixture of water and ethyl ether. The organic layer is separated, washed three times with portions of water and dried over anhydrous sodium sulfate. The solvents are removed under reduced pressure to give 1-ethoxycarbonyl-4-decylpiperazine. refluxed for approximately 44 hours under a nitrogen atmosphere The organic layer is separated washed three times with portions of water dried over anhydrous sodium sulfate The solvents are removed under reduced pressure

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

実験手順: To a cooled solution of 158.3 grams of 1-decanol in 1.0 liter of collidine is added dropwise 126 grams of mesyl chloride. The resulting mixture is stirred at room temperature for 1.5 hours and then poured onto ice. The reaction mixture is extracted with ether and the ether extracts are washed with 10% hydrochloric acid. The ether extracts are combined, dried over anhydrous sodium sulfate, and the solvent removed under reduced pressure to leave an oil which solidifies upon cooling. The oil is dissolved in n-hexane and cooled to yield as crystals, decyl methylsulfonate. poured onto ice The reaction mixture is extracted with ether the ether extracts are washed with 10% hydrochloric acid dried over anhydrous sodium sulfate the solvent removed under reduced pressure to leave an oil which upon cooling cooled

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

実験手順: To a cooled solution of 158.3 grams of 1-decanol in 1.0 liter of collidine is added dropwise 126 grams of mesyl chloride. The resulting mixture is stirred at room temperature for 1.5 hours and then poured onto ice. The reaction mixture is extracted with ether and the ether extracts are washed with 10% hydrochloric acid. The ether extracts are combined, dried over anhydrous sodium sulfate, and the solvent removed under reduced pressure to leave an oil which solidifies upon cooling. The oil is dissolved in n-hexane and cooled to yield as crystals, decyl methylsulfonate. poured onto ice The reaction mixture is extracted with ether the ether extracts are washed with 10% hydrochloric acid dried over anhydrous sodium sulfate the solvent removed under reduced pressure to leave an oil which upon cooling cooled

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

実験手順: 77.3 Grams of decyl methylsulfonate, 44.64 grams of 1-ethoxycarbonylpiperazine, 500 ml. of ethanol, and 39 grams of potassium carbonate are combined and refluxed for approximately 44 hours under a nitrogen atmosphere. After cooling to room temperature the residue is dissolved in a mixture of water and ethyl ether. The organic layer is separated, washed three times with portions of water and dried over anhydrous sodium sulfate. The solvents are removed under reduced pressure to give 1-ethoxycarbonyl-4-decylpiperazine. refluxed for approximately 44 hours under a nitrogen atmosphere The organic layer is separated washed three times with portions of water dried over anhydrous sodium sulfate The solvents are removed under reduced pressure

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

実験手順: To a cooled solution of 158.3 grams of 1-decanol in 1.0 liter of collidine is added dropwise 126 grams of mesyl chloride. The resulting mixture is stirred at room temperature for 1.5 hours and then poured onto ice. The reaction mixture is extracted with ether and the ether extracts are washed with 10% hydrochloric acid. The ether extracts are combined, dried over anhydrous sodium sulfate, and the solvent removed under reduced pressure to leave an oil which solidifies upon cooling. The oil is dissolved in n-hexane and cooled to yield as crystals, decyl methylsulfonate. poured onto ice The reaction mixture is extracted with ether the ether extracts are washed with 10% hydrochloric acid dried over anhydrous sodium sulfate the solvent removed under reduced pressure to leave an oil which upon cooling cooled

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: Ethyl 1-piperazinecarboxylate (77.3 g, 0.28 mole), 1-decanol methanesulfonate (77.3 g, 0.28 mole) from the condensation of 1-decanol with methane sulfonyl chloride, K2CO3 (39.0 g, 0.28 mole), and 500 mL of EtOH were combined and refluxed for 2 days under N2. After cooling to room temperature, the reaction was partitioned between water and Et2O. The organic layer was separated, washed 3 times with water, dried over Na2SO4 and stripped of all solvent under reduced pressure to yield the crude product oil. Chromatographic purification of the crude oil gave 53.4 g of ethyl 4-decyl-1-piperazinecarboxylate. refluxed for 2 days under N2 the reaction was partitioned between water and Et2O The organic layer was separated washed 3 times with water dried over Na2SO4 to yield the crude product oil Chromatographic purification of the crude oil

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

実験手順: Ethyl 1-piperazinecarboxylate (77.3 g, 0.28 mole), 1-decanol methanesulfonate (77.3 g, 0.28 mole) from the condensation of 1-decanol with methane sulfonyl chloride, K2CO3 (39.0 g, 0.28 mole), and 500 mL of EtOH were combined and refluxed for 2 days under N2. After cooling to room temperature, the reaction was partitioned between water and Et2O. The organic layer was separated, washed 3 times with water, dried over Na2SO4 and stripped of all solvent under reduced pressure to yield the crude product oil. Chromatographic purification of the crude oil gave 53.4 g of ethyl 4-decyl-1-piperazinecarboxylate. refluxed for 2 days under N2 the reaction was partitioned between water and Et2O The organic layer was separated washed 3 times with water dried over Na2SO4 to yield the crude product oil Chromatographic purification of the crude oil

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

実験手順: Ethyl 1-piperazinecarboxylate (77.3 g, 0.28 mole), 1-decanol methanesulfonate (77.3 g, 0.28 mole) from the condensation of 1-decanol with methane sulfonyl chloride, K2CO3 (39.0 g, 0.28 mole), and 500 mL of EtOH were combined and refluxed for 2 days under N2. After cooling to room temperature, the reaction was partitioned between water and Et2O. The organic layer was separated, washed 3 times with water, dried over Na2SO4 and stripped of all solvent under reduced pressure to yield the crude product oil. Chromatographic purification of the crude oil gave 53.4 g of ethyl 4-decyl-1-piperazinecarboxylate. refluxed for 2 days under N2 the reaction was partitioned between water and Et2O The organic layer was separated washed 3 times with water dried over Na2SO4 to yield the crude product oil Chromatographic purification of the crude oil

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

実験手順: Ethyl 1-piperazinecarboxylate (77.3 g, 0.28 mole), 1-decanol methanesulfonate (77.3 g, 0.28 mole) from the condensation of 1-decanol with methane sulfonyl chloride, K2CO3 (39.0 g, 0.28 mole), and 500 mL of EtOH were combined and refluxed for 2 days under N2. After cooling to room temperature, the reaction was partitioned between water and Et2O. The organic layer was separated, washed 3 times with water, dried over Na2SO4 and stripped of all solvent under reduced pressure to yield the crude product oil. Chromatographic purification of the crude oil gave 53.4 g of ethyl 4-decyl-1-piperazinecarboxylate. refluxed for 2 days under N2 the reaction was partitioned between water and Et2O The organic layer was separated washed 3 times with water dried over Na2SO4 to yield the crude product oil Chromatographic purification of the crude oil