反应详情

温度

80 °C

A mixture of 1-(2-chloropyridin-3-yl)propane-1,3-diol (62.9 mmol) and KOtBu (189 mmol) in 240 mL tBuOH (dried over 3 Å molsieves) was heated to 80° C. for 2.5 h. The reaction mixture was then concentrated to about ¼ of its volume, diluted with water and extracted 5 times with DCM. The combined organic layers were washed with brine, dried over MgSO4 and concentrated in vacuo. Purification with CC (KP-SIL™ from Biotage) using MeOH/DCM (99/1 to 95/5) gives the desired compound as orange oil.

1. concentrationThe reaction mixture was then concentrated to about ¼ of its volume
2. additiondiluted with water
3. extractionextracted 5 times with DCM
4. washThe combined organic layers were washed with brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. customPurification with CC (KP-SIL™ from Biotage)