1-(2-methoxyethyl)piperazine;dihydrochloride

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

実験手順: To a suspension of 1-(2-methoxyethyl)piperazine dihydrochloride (2.61 g, 12.0 mmol) in THF (100 mL) was added triethylamine (10 mL) and the resulting mixture was stirred for 10 min. Then a solution of 2-thiophenesulfonyl chloride (1.98 g, 10.84 mmol) was added in THF (3 mL) over 5 min. The reaction mixture was allowed to stir at room temperature for 1 h, the volatiles were evaporated and the residue was extracted with ethyl acetate (3×100 mL). The combined extracts were washed with a saturated sodium bicarbonate solution (50 mL), brine and dried over molecular sieves. Evaporation to dryness gave a viscous oil (2.09 g, 75%). to stir at room temperature for 1 h the volatiles were evaporated the residue was extracted with ethyl acetate (3×100 mL) The combined extracts were washed with a saturated sodium bicarbonate solution (50 mL), brine dried over molecular sieves Evaporation to dryness

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

実験手順: To a suspension of 1-(2-methoxyethyl)piperazine dihydrochloride (2.61 g, 12.0 mmol) in THF (100 mL) was added triethylamine (10 mL) and the resulting mixture was stirred for 10 min. Then a solution of 2-thiophenesulfonyl chloride (1.98 g, 10.84 mmol) was added in THF (3 mL) over 5 min. The reaction mixture was allowed to stir at room temperature for 1 h, the volatiles were evaporated and the residue was extracted with ethyl acetate (3×100 mL). The combined extracts were washed with a saturated sodium bicarbonate solution (50 mL), brine and dried over molecular sieves. Evaporation to dryness gave a viscous oil (2.09 g, 75%). to stir at room temperature for 1 h the volatiles were evaporated the residue was extracted with ethyl acetate (3×100 mL) The combined extracts were washed with a saturated sodium bicarbonate solution (50 mL), brine dried over molecular sieves Evaporation to dryness

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

実験手順: To an aqueous solution of 68.8 g of 1-(2-methoxyethyl)piperazine dihydrochloride (water; 50 mL) was added dropwise an aqueous solution of 33.0 g of sodium hydroxide (water; 100 mL). The mixture was extracted with chloroform. The, organic layer was dried over anhydrous magnesium sulfate and evaporated to give 41.3 g of the title compound. The mixture was extracted with chloroform The, organic layer was dried over anhydrous magnesium sulfate evaporated

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

実験手順: To a solution of 57.2 g of 1-formyl-4-methoxyethylpiperazine in 100 mL of methanol was added dropwise 180 mL of 4N-hydrochloric acid/1,4-dioxane over 1.5 hours. The mixture was stirred at room temperature for 1 hour, and the resulting crystals were filtered, washed with isopropyl ether and dried in vacuo to give 68.8 g of the title compound. the resulting crystals were filtered washed with isopropyl ether dried in vacuo