反应详情

温度

0 °C

Add DBU (240 mg, 1.55 mmol) to a solution of 5-hydroxymethyl-2-(3-methyl-butyryl)-pyridine (250 mg, 1.29 mmol) and diphenylphosphorylazide (430 mg, 1.55 mmol) in anhydrous toluene (10 mL) at 0° C. Stir at 0° C. for 30 min, warm to room temperature and stir for 4 h. Dilute with EtOAc and water. Extract the aqueous phase twice with EtOAc. Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo. Purify the crude mixture by chromatography on silica gel eluting with hexane and hexane/EtOAc (9:1) to provide the desired intermediate (300 mg, 99%). MS (ES+) m/z: 219 (M+H)+.

1. temperaturewarm to room temperature
2. stirringstir for 4 h
3. extractionExtract the aqueous phase twice with EtOAc
4. dry with materialDry the combined organic extracts over Na2SO4
5. filtrationfilter
6. concentrationconcentrate in vacuo
7. customPurify the crude mixture by chromatography on silica gel eluting with hexane and hexane/EtOAc (9:1)