反应详情

温度

0 °C

Methyl 5,6-dichloronicotinate (1.5 g) and 60% sodium hydride (640 mg) were dissolved in THF (45 mL). 1,3-Difluoropropan-2-ol (1.5 g) was added thereto at 0° C., followed by stirring at 0° C. for 3 hours, and the reaction solution was quenched with aqueous NH4Cl. After extraction with EtOAc, the organic layer was dried over MgSO4 and then filtered, and the desiccant was removed. The vehicle was evaporated under reduced pressure, followed by purification by silica gel column chromatography (hexane:AcOEt=100:0 to 50:50) to obtain methyl 5-chloro-6-[(1,3-difluoropropan-2-yl)oxy]nicotinate (1.56 g) as a colorless liquid.

1. customat 0° C.
2. customthe reaction solution was quenched with aqueous NH4Cl
3. extractionAfter extraction with EtOAc
4. dry with materialthe organic layer was dried over MgSO4
5. filtrationfiltered
6. customthe desiccant was removed
7. customThe vehicle was evaporated under reduced pressure
8. customfollowed by purification by silica gel column chromatography (hexane:AcOEt=100:0 to 50:50)