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温度

0 °C

A mixture of 2-(3,4-dimethoxy-phenyl)-N-[3-(3,4-dimethoxy-phenyl)-propyl]-acetamide (6.16 g, 16.49 mmol) and POCl3 (4.95 ml, 54.07 mmol) in anhydrous acetonitrile (185 ml) was stirred at reflux for 4 h under nitrogen. After cooling, the reaction mixture was concentrated in vacuo and the residue was dissolved in MeOH (125 ml). The solution was cooled to 0° C. and NaBH4 (4.31 g, 113.93 mmol) was added portionwise. After stirring at 0° C. for 2 h under nitrogen, the reaction mixture was poured into H2O and extracted three times with CH2Cl2. The combined organic extracts were washed with brine, dried over anhydrous MgSO4, filtered and concentrated to give a crude oil. Flash chromatography (CH2Cl2/MeOH: 9/1) gave the title compound as a racemic mixture (2.29 g, 6.40 mmol, 39%, yellow oil).

1. temperatureat reflux for 4 h under nitrogen
2. temperatureAfter cooling
3. concentrationthe reaction mixture was concentrated in vacuo
4. dissolutionthe residue was 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 were washed with brine
8. dry with materialdried over anhydrous MgSO4
9. filtrationfiltered
10. concentrationconcentrated
11. customto give a crude oil