反应详情

温度

100 °C

2,6-Dimethyl-pyridin-4-ol 10I (6.16 g, 50 mmol), PBr5 (11.9 g, 27.65 mmol) and POBr3 (2.5 mL, 24.6 mmol) was combined and CHCl3 (2.5 mL) was added. The reaction was heated at 100° C. for 5 hrs and then cooled in an ice bath. Solid KOH was added till PH reached 7-8 followed by extraction with Et2O (3×75 mL). The combined ether layer was dried and evaporated in vacuo to give a thick clear crude oil (10.1 g) as the title compound.

1. temperaturecooled in an ice bath
2. extractionfollowed by extraction with Et2O (3×75 mL)
3. dry with materialThe combined ether layer was dried
4. customevaporated in vacuo