反应详情

温度

0 °C

Under argon and in an anhydrous medium, 730 μl (7.95 mmol) of phosphorus oxychloride are added dropwise to 12.5 ml of N,N-dimethylformamide maintained at 0° C.; after 30 minutes' stirring, 1.50 g (5.3 mmol) of the compound obtained in Step A dissolved in 25 ml of N,N-dimethylformamide are added by transfer. The reaction, mixture is stirred for 30 minutes at 0° C. and then for 3 hours at room temperature. The reaction mixture is evaporated to dryness and then taken up in water; the aqueous phase is rendered alkaline with a 6N sodium hydroxide solution and extracted several times with ethyl acetate. The combined organic phases are dried over magnesium sulphate, filtered and then evaporated. After washing with a petroleum ether/diethyl ether mixture, the title compound is obtained in the form of a yellow oil.

1. additionare added by transfer
2. customThe reaction, mixture
3. stirringis stirred for 30 minutes at 0° C.
4. waitfor 3 hours at room temperature
5. customThe reaction mixture is evaporated to dryness
6. extractionextracted several times with ethyl acetate
7. dry with materialThe combined organic phases are dried over magnesium sulphate
8. filtrationfiltered
9. customevaporated
10. washAfter washing with a petroleum ether/diethyl ether mixture