反应详情

Dissolve (S)-1-(3,5-dichloropyridin-4-yl)ethanol (5.02 g, 26.14 mmol) in dichloromethane (DCM, 100 mL) and cool the flask in an ice bath. Add triethylamine (TEA, 3.5 mL, 25.11 mmol) followed by the dropwise addition of methanesulfonyl chloride (2.2 mL, 28.42 mmol). Remove the ice bath and allow the reaction to warm to RT. After 4 hours, quench the reaction with water (100 mL) and separate layers. Extract the aqueous layer with DCM (50 mL) followed by 20% isopropyl alcohol (IPA)/chloroform (50 mL). Combine the organic extracts, dry over anhydrous sodium sulfate, filter and concentrate in vacuo. Yield: 7.15 g, (100%). MS (ES) m/z 270 [M+1]+.

1. temperaturecool the flask in an ice bath
2. customRemove the ice bath
3. customthe reaction
4. customquench
5. customthe reaction with water (100 mL)
6. customseparate layers
7. extractionExtract the aqueous layer with DCM (50 mL)
8. dry with materialCombine the organic extracts, dry over anhydrous sodium sulfate
9. filtrationfilter
10. concentrationconcentrate in vacuo