反应详情

From a reaction system containing 3-Azidomethyl-5-fluoromethylbenzylalcohol (36) (142 mg, 0.73 mmol), the air was evacuated and then Ar was charged therein. To this were added DMTrCl (323 mg, 0.95 mmol), DMF (2.0 mL), and pyridine (2.0 mL), and stirred for 22 hours at a room temperature. TLC was used to confirm the progress of the reaction. Then, the solvent was removed in vacuo. The residue was subjected to extraction with EtOAc. The organic layer was washed with a saturated sodium chloride aqueous solution, dried over anhydrous sodium sulfate, and evaporated under reduced pressure to remove the solvent. The residue was purified by neutral silica gel column chromatography (hexane:EtOAc=20:1 to 5:1) to isolate

1. customthe air was evacuated
2. additionAr was charged
3. customthe progress of the reaction
4. customThen, the solvent was removed in vacuo
5. extractionThe residue was subjected to extraction with EtOAc
6. washThe organic layer was washed with a saturated sodium chloride aqueous solution
7. dry with materialdried over anhydrous sodium sulfate
8. customevaporated under reduced pressure
9. customto remove the solvent
10. customThe residue was purified by neutral silica gel column chromatography (hexane:EtOAc=20:1 to 5:1)
11. customto isolate