反应详情

温度

0 °C

A mixture of 2-(3,4-dimethoxy-phenyl)-N-[3-(3,4-dimethoxy-phenyl)-propyl]-acetamide (6.16 g, 16.5 mmol) and POCl3 (4.95 mL, 54.1 mmol) in anhydrous acetonitrile (185 mL) is stirred at reflux for 4 h under nitrogen. After cooling, the reaction mixture is evaporated and the residue is dissolved in MeOH (125 mL). The solution is cooled to 0° C. and NaBH4 (4.31 g, 114 mmol) is added portionwise. After stirring at 0° C. for 2 h under nitrogen, the reaction mixture is poured into H2O and extracted three times with CH2Cl2. The combined organic extracts are washed with brine, dried over anhydrous MgSO4, filtered and concentrated to give a crude oil. Flash chromatography (CH2Cl2/MeOH: 9/1) yields the title compound as a yellow oil.

1. temperatureat reflux for 4 h under nitrogen
2. temperatureAfter cooling
3. customthe reaction mixture is evaporated
4. dissolutionthe residue is dissolved in MeOH (125 mL)
5. stirringAfter stirring at 0° C. for 2 h under nitrogen
6. extractionextracted three times with CH2Cl2
7. washThe combined organic extracts are washed with brine
8. dry with materialdried over anhydrous MgSO4
9. filtrationfiltered
10. concentrationconcentrated
11. customto give a crude oil