反应详情

温度

0 °C

A mixture of 2-(1,3-dioxolan-2-yl)-1-(6-(trifluoromethyl)pyridin-3-yl)ethanol (18.54 g, 0.070 mol) and diphenylphosphonic azide (36 mL, 0.17 mol) in toluene (40 mL) was cooled to 0° C. and neat 1,8-diazabicyclo[5.4.0]undec-7-ene (25 mL, 0.17 mol) was added. The reaction mixture was stirred at 0° C. for 2 hr and then at 20° C. overnight. The mixture was washed with water and 5% HCl. The aqueous phase was extracted with CH2Cl2. The combined orangic layers were concentrated in vacuo and the residue was purified by silica gel column (0-100% EtOAc/hexane) to afford a colorless oil.

1. customat 20° C.
2. customovernight
3. washThe mixture was washed with water and 5% HCl
4. extractionThe aqueous phase was extracted with CH2Cl2
5. concentrationThe combined orangic layers were concentrated in vacuo
6. customthe residue was purified by silica gel column (0-100% EtOAc/hexane)
7. customto afford a colorless oil