反应详情

A mixture of phosphorus oxychloride (1.93 ml, 0.02 mmol) and [1-(2,3-dihydrobenzo[1,4]dioxin-2-ylmethyl)-3-methylpiperidin-3-yl]methanol (0.2 g, 0.72 mmol) was refluxed for 3 h. Excess of phosphorus oxychloride was evaporated. Water was slowly added and the reaction mixture was made alkaline with aq NaOH and extracted with DCM (3×5 ml). The combined organic phases were dried over Na2SO4, filtered and the filtrate was evaporated to give the title compound, which was purified by column chromatography (DCM/MeOH, 90:10).

1. temperaturewas refluxed for 3 h
2. customExcess of phosphorus oxychloride was evaporated
3. additionWater was slowly added
4. extractionextracted with DCM (3×5 ml)
5. dry with materialThe combined organic phases were dried over Na2SO4
6. filtrationfiltered
7. customthe filtrate was evaporated