反应详情

温度

-78 °C

Combine 2-pyrrolidinone (0.39 g, 4.62 mmol) and tetrahydrofuran (5 mL). Cool to −78° C. using a dry-ice/acetone bath. Add a solution of sec-butyl lithium (4.3 mL, 1.3 M in hexane, 5.55 mmol). After 15 minutes, add a solution of 3,4,5-trimethoxybenzyl chloride (1.00 g, 4.62 mmol) in tetrahydrofuran (5 mL). After the addition of 3,4,5-trimethoxybenzyl chloride is complete, heat to reflux. After 12 hours, cool the reaction mixture and partition between water and ethyl acetate. Separate the aqueous layer and extract 4 times with ethyl acetate. Dry the combined organic layers over Na2SO4, filter, and concentrate in vacuo to give the title compound.

1. temperatureheat to reflux
2. waitAfter 12 hours
3. temperaturecool the reaction mixture
4. custompartition between water and ethyl acetate
5. customSeparate the aqueous layer
6. extractionextract 4 times with ethyl acetate
7. dry with materialDry the combined organic layers over Na2SO4
8. filtrationfilter
9. concentrationconcentrate in vacuo