反应详情

0.27 ml (1.92 mmol) of triethylamine and 165 mg (1.44 mmol) of methanesulfonyl chloride were added to 5 ml of dichloromethane containing 360 mg (0.96 mmol) of t-butyl [(1S)-2-hydroxy-1-(4-iodobenzyl)ethyl]carbamate under cooling with ice. After stirring for 30 minutes, the temperature was elevated to room temperature, and the mixture was stirred for 15 hours. The reaction liquid was diluted with water. After the extraction with dichloromethane, the organic layer was successively washed with 1 N hydrochloric acid, 1 N sodium hydroxide and saturated aqueous NaCl solution, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. 10 ml of dimethylformamide and 203 mg (4.8 mmol) of lithium chloride were added to the residue, and they were stirred at 50° C. for 19 hours. The reaction liquid was diluted with water. After the extraction with ethyl acetate, the organic layer was successively washed with water and saturated aqueous NaCl solution. The solvent was evaporated, and the residue was purified by the silica gel column chromatography to obtain the title compound.

1. temperatureunder cooling with ice
2. customwas elevated to room temperature
3. stirringthe mixture was stirred for 15 hours
4. customThe reaction liquid
5. extractionAfter the extraction with dichloromethane
6. washthe organic layer was successively washed with 1 N hydrochloric acid, 1 N sodium hydroxide and saturated aqueous NaCl solution
7. dry with materialdried over anhydrous magnesium sulfate
8. customThe solvent was evaporated under reduced pressure
9. stirringwere stirred at 50° C. for 19 hours
10. customThe reaction liquid
11. extractionAfter the extraction with ethyl acetate
12. washthe organic layer was successively washed with water and saturated aqueous NaCl solution
13. customThe solvent was evaporated
14. customthe residue was purified by the silica gel column chromatography