反应详情

温度

105 °C

Into a Schlenk flask equipped with a magnetic stir bar was added 1-difluoromethyl-7-iodo-1-methyl-1,2,3,4-tetrahydro-benzofuro[2,3-C]pyridine (enantiomer 1, 100 mg, 0.30 mmol), (2,3-difluorophenylsulfanyl)-triisopropylsilane (125 mg, 0.43 mmol), CsF (189 mg, 1.24 mmol), CuI (25 mg, 0.13 mmol), ethylene glycol (85 μL, 1.5 mmol) and anhydrous DMF (3 mL, 0.30 mmol). The Schlenck flask was evacuated and flushed with argon three times. The reaction mixture was heated at 105° C. under argon for 17 h. Upon cooling, the reaction was diluted with DCM, filtered through celite and solvent was evaporated. Purification using preparative TLC (2000 micron silica gfel plate; elution with 15% EtOAc in dichloromethane) afforded 155 mg of product as a viscous, pale oil. MS m/z: 382 [M+H]+.

1. customInto a Schlenk flask equipped with a magnetic stir bar
2. customThe Schlenck flask was evacuated
3. customflushed with argon three times
4. temperatureUpon cooling
5. additionthe reaction was diluted with DCM
6. filtrationfiltered through celite and solvent
7. customwas evaporated
8. customPurification
9. washTLC (2000 micron silica gfel plate; elution with 15% EtOAc in dichloromethane)