6-methylsulfonyloxyhexyl methanesulfonate

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

実験手順: At 70° C., under nitrogen, a mixture of 137 g of 1,6-hexanediyl dimethanesulfonate and 175.5 g of cysteine-hydrochloride monohydrated in 1.5 l of water containing a little ethanol is agitated. There is then slowly added a solution of 5 N NaOH so that the pH of the reaction mixture is maintained between 8.5 and 9.5. At the end of the reaction the mixture is acidified to pH 5.2 with a solution of HCl. The precipitate is filtered, washed thoroughly with water, then dried and analyzed. is maintained between 8.5 and 9.5 At the end of the reaction the mixture The precipitate is filtered washed thoroughly with water dried

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

実験手順: At 70° C., under nitrogen, a mixture of 137 g of 1,6-hexanediyl dimethanesulfonate and 175.5 g of cysteine-hydrochloride monohydrated in 1.5 l of water containing a little ethanol is agitated. There is then slowly added a solution of 5 N NaOH so that the pH of the reaction mixture is maintained between 8.5 and 9.5. At the end of the reaction the mixture is acidified to pH 5.2 with a solution of HCl. The precipitate is filtered, washed thoroughly with water, then dried and analyzed. is maintained between 8.5 and 9.5 At the end of the reaction the mixture The precipitate is filtered washed thoroughly with water dried

反応条件: temp:5.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 1,6-hexanediol (13.15 g, 111.3 mmol) in 70 mL of anhydrous pyridine was cooled to 0° C. using ice bath. To this methanesulfonyl chloride (27 g, 235.7 mmol) was slowly added under mixing such that the temperature was maintained at 5-6° C. The combined mixture was stirred overnight at the temperature below 10° C. and the precipitate formed was filtered off, washed with 20% HCl (3×), water (3×), 5% solution of sodium bicarbonate (3×), and then again with water (3×). Product was dried under vacuum to obtain Compound 1 as a white solid (yield 32.8%). The structure of Compound 1 is given below: under mixing such that the temperature the precipitate formed was filtered off washed with 20% HCl (3×), water (3×), 5% solution of sodium bicarbonate (3×) Product was dried under vacuum

反応条件: temp:5.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 1,6-hexanediol (13.15 g, 111.3 mmol) in 70 mL of anhydrous pyridine was cooled to 0° C. using ice bath. To this methanesulfonyl chloride (27 g, 235.7 mmol) was slowly added under mixing such that the temperature was maintained at 5-6° C. The combined mixture was stirred overnight at the temperature below 10° C. and the precipitate formed was filtered off, washed with 20% HCl (3×), water (3×), 5% solution of sodium bicarbonate (3×), and then again with water (3×). Product was dried under vacuum to obtain Compound 1 as a white solid (yield 32.8%). The structure of Compound 1 is given below: under mixing such that the temperature the precipitate formed was filtered off washed with 20% HCl (3×), water (3×), 5% solution of sodium bicarbonate (3×) Product was dried under vacuum

反応条件: temp:5.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 1,6-hexanediol (13.15 g, 111.3 mmol) in 70 mL of anhydrous pyridine was cooled to 0° C. using ice bath. To this methanesulfonyl chloride (27 g, 235.7 mmol) was slowly added under mixing such that the temperature was maintained at 5-6° C. The combined mixture was stirred overnight at the temperature below 10° C. and the precipitate formed was filtered off, washed with 20% HCl (3×), water (3×), 5% solution of sodium bicarbonate (3×), and then again with water (3×). Product was dried under vacuum to obtain Compound 1 as a white solid (yield 32.8%). The structure of Compound 1 is given below: under mixing such that the temperature the precipitate formed was filtered off washed with 20% HCl (3×), water (3×), 5% solution of sodium bicarbonate (3×) Product was dried under vacuum

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

実験手順: At 70° C., under nitrogen, a mixture of 137 g of 1,6-hexanediyl dimethanesulfonate and 175.5 g of cysteine-hydrochloride monohydrated in 1.5 l of water containing a little ethanol is agitated. There is then slowly added a solution of 5 N NaOH so that the pH of the reaction mixture is maintained between 8.5 and 9.5. At the end of the reaction the mixture is acidified to pH 5.2 with a solution of HCl. The precipitate is filtered, washed thoroughly with water, then dried and analyzed. is maintained between 8.5 and 9.5 At the end of the reaction the mixture The precipitate is filtered washed thoroughly with water dried