反应详情

温度

40 °C

To a solution of (3S)-4-(4,6-dichloropyrimidin-2-yl)-3-methylmorpholine (992 mg, 4.0 mmol) in THF (20 mL) was added n-butyllithium (1.56 mL, 1.6 M) dropwise at −78° C. and the mixture was stirred for 30 min. 1,3,2-dioxathiolane 2,2-dioxide (672 mg, 5.41 mmol) was added, and stirring was continued for 30 min, whereupon 6 N HCl (13.3 mL) was added. The reaction mixture was stirred for 18 h and then heated at 40° C. for 4 h. The reaction mixture was extracted with ethyl acetate, and the organic layer was washed with brine, dried with MgSO4, filtered and concentrated by rotary evaporation.

1. stirringstirring
2. additionwas added
3. stirringThe reaction mixture was stirred for 18 h
4. extractionThe reaction mixture was extracted with ethyl acetate
5. washthe organic layer was washed with brine
6. dry with materialdried with MgSO4
7. filtrationfiltered
8. concentrationconcentrated by rotary evaporation