反应详情

Under ice-cooling, oxalyl chloride (0.27 mL) was added dropwise into a dichloromethane (5 mL) solution containing 1-[(3S,5R)-5-(3,4,5-trifluorophenyl)morpholin-3-yl]ethanol (269 mg) and pyridine (5 mL). Stirring was continued for 30 minutes at the same temperature and for 1 hour at room temperature. Water was added, and the organic layer was partitioned, and the resultant was dried over anhydrous magnesium sulfate. The solvent was removed under a vacuum, and the resultant was purified by silica gel column chromatography (heptane/ethyl acetate→ethyl acetate), and the title compound (136 mg) was obtained. The physical property values are as follows.

1. temperatureUnder ice-cooling
2. customthe organic layer was partitioned
3. dry with materialthe resultant was dried over anhydrous magnesium sulfate
4. customThe solvent was removed under a vacuum
5. customthe resultant was purified by silica gel column chromatography (heptane/ethyl acetate→ethyl acetate)