反应详情

温度

-70 °C

Tetrahydrofuran (100 ml) and 1,3-dimethyl-3,4,5,6-tetrahydro 2 (1H)-pyrimidinone (140 ml) were mixed at −20° C. and lithium bis (trimethylsilyl) amide (1M in tetrahydrofuran, 100 ml) was added. The mixture was cooled to −70° C., ethyl isovalerate (18.75 ml) added and stirred for ½ hour at −70° C. Triisopropylsilyl trifluoromethane sulfonate was added and the mixture left to stir at −75° C. for ½ hour before warming to room temperature and stirring for 3 hours. The reaction mixture was quenched with aqueous sodium bicarbonate (8%, 150 ml) and extracted with hexane (1000 ml). The hexane extract was washed with water (4×500 ml), dried (MgSO4), filtered and concentrated in vacuo to afford a crude yellow oil containing the title compound.

1. waitthe mixture left
2. stirringto stir at −75° C. for ½ hour
3. temperaturebefore warming to room temperature
4. stirringstirring for 3 hours
5. customThe reaction mixture was quenched with aqueous sodium bicarbonate (8%, 150 ml)
6. extractionextracted with hexane (1000 ml)
7. extractionThe hexane extract
8. washwas washed with water (4×500 ml)
9. dry with materialdried (MgSO4)
10. filtrationfiltered
11. concentrationconcentrated in vacuo
12. customto afford a crude yellow oil