methyl thiomorpholine-3-carboxylate;hydrochloride

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

実験手順: 20 g (0.085 mol) methyl 2-chloroethyl cysteine hydrochloride was dissolved with 200 ml water, and a solution of 7.2 g (0.085 mol) sodium bicarbonate dissolved in 120 ml water was added dropwise to the above-obtained solution under ice bath condition, and then the mixed solution was allowed to react by keeping a constant temperature in the bath ice for 1 hour. The obtained reaction product was extracted with ethyl acetate (100 ml×3), and the resulting ester layers were combined, and dried with anhydrous sodium sulfate for 4 hours. The solvent was removed by evaporation under reduced pressure. The resulting residue was dissolved with 400 ml anhydrous methanol, and reacted with stirring at room temperature for 5 days, followed by removing solvent by evaporation under reduced pressure. The resulting residue was recrystallized with anhydrous methanol/ethyl acetate, obtaining 8.9 g of a white crystal, yield 49.2%. was added dropwise to the above-obtained solution under ice bath condition to react for 1 hour The obtained reaction product was extracted with ethyl acetate (100 ml×3) dried with anhydrous sodium sulfate for 4 hours The solvent was removed by evaporation under reduced pressure The resulting residue was dissolved with 400 ml anhydrous methanol reacted by removing solvent by evaporation under reduced pressure The resulting residue was recrystallized with anhydrous methanol/ethyl acetate