反应详情

温度

5 °C

Phosphorous oxychloride (145 g, 0.95 mol) was added dropwise at 5° C. to 280 mL of stirred N,N-dimethylformamide (DMF), and the mixture was stirred at 5° C. for 2 hours. N-(6-Acetoxyhexyl)-N-methylaniline (Example 2, 230 g, 0.93 mol) was added slowly, and the reaction mixture was heated at 90° C. for 3 hours. After cooling, the solution was poured onto 500 g of ice and the resulting mixture was neutralized to pH 5 with sodium acetate. The mixture was extracted with dichloromethane (4×200 mL), the combined extracts were dried (MgSO4), and the solvent was removed at reduced pressure. The brown residue was distilled in vacuo to provide 186 g (73%) of a yellow oil, bp 195° C. (0.15 mm).

1. temperaturethe reaction mixture was heated at 90° C. for 3 hours
2. temperatureAfter cooling
3. extractionThe mixture was extracted with dichloromethane (4×200 mL)
4. dry with materialthe combined extracts were dried (MgSO4)
5. customthe solvent was removed at reduced pressure
6. distillationThe brown residue was distilled in vacuo