反应详情

温度

60 °C

To a solution of ethyl 4-[(2-chloro-4,4-difluoro-spiro[5H-thieno[2,3-c]pyran-7,4′-piperidine]-1′-yl)methyl]-1H-pyrazole-3-carboxylate (22.5 g, 52.10 mmoles) in Dimethylformamide (225.00 mL) is added Potassium Carbonate (10.80 g, 78.14 mmoles) and 2,3-difluoropyridine (7.19 g, 62.52 mmoles) and the resulting suspension is stirred at 60° C. 15 h. Then, reaction mixture is poured over Ice/brine (30 mL) and CH2Cl2 (50 mL) is added to the resulting suspension. Solution is washed with H2O (2×50 mL). Organics are dried over sodium sulfate and concentrated to give a crude which is purified via SiO2 filtration eluting with 2-propanol/CH2Cl2 mixtures to give 18 g of the title compound. MS (m/z): 527 (M+1).

1. custom15 h
2. customThen, reaction mixture
3. additionis added to the resulting suspension
4. washSolution is washed with H2O (2×50 mL)
5. dry with materialOrganics are dried over sodium sulfate
6. concentrationconcentrated
7. customto give a crude which
8. filtrationis purified via SiO2 filtration
9. washeluting with 2-propanol/CH2Cl2