反应详情

温度

55 °C

To a mixture of the crude azide (330 mg, 1.33 mmol) in THF (12 mL) were added polymer-supported Ph3P (2.0 eq.) and water (2 mL). The reaction mixture was stirred at 55° C. until completion of the reaction, cooled down to rt and filtered. The filtrate was partitioned between EA and aq. sat. NaHCO3 and the layers separated. The aq. layer was extracted with EA and the combined org. extracts dried over MgSO4, filtered and concentrated under reduced pressure to give the title compound as a yellow solid. LC-MS-conditions 02: tR=0.54 min; [M+CH3CN+H]+=263.45.

1. temperaturecooled down to rt
2. filtrationfiltered
3. customThe filtrate was partitioned between EA and aq. sat. NaHCO3
4. customthe layers separated
5. extractionThe aq. layer was extracted with EA
6. dry with materialextracts dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure