反应详情

In 130 ml of anhydrous acetone was dissolved 13.24.g of trans-N-t-butoxycarbonyl-4-methanesulfonyloxymethylcyclohexylmethylamine, and 12.32 g of sodium iodide was added thereto, and the resulting mixture was heated under reflux for 3 hours and 45 minutes. The solvent was distilled off under reduced pressure and the residue was dissolved in ethyl acetate. The resulting solution was washed successively with an aqueous sodium thiosulfate solution and an aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (eluting solvent: cyclohexane/ethyl acetate=4/1) to obtain a pale yellow crystalline solid. The crystalline solid was recrystallized from hexane to obtain 13.67 g of the desired compound as a colorless crystalline solid.

1. additionwas added
2. temperaturethe resulting mixture was heated
3. temperatureunder reflux for 3 hours and 45 minutes
4. distillationThe solvent was distilled off under reduced pressure
5. dissolutionthe residue was dissolved in ethyl acetate
6. washThe resulting solution was washed successively with an aqueous sodium thiosulfate solution
7. dry with materialan aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate
8. distillationThe solvent was distilled off under reduced pressure
9. customthe residue was purified by silica gel column chromatography (eluting solvent: cyclohexane/ethyl acetate=4/1)
10. customto obtain a pale yellow crystalline solid
11. customThe crystalline solid was recrystallized from hexane