反应详情

A mixture of 1-(4-bromo-3-fluorophenyl)cyclopropanecarboxylic acid (7.4 g, 28.6 mmol, prepared from 1-bromo-4-bromomethyl-2-fluorobenzene according to Peretto et al. J Med. Chem. 2005, 48, 5705-20), DIPEA (6.36 mL, 37.1 mmol), tert-butanol (67.0 mL, 714 mmol), diphenylphosphorylazide (7.37 mL, 34.3 mmol) and molsieve (4 Å) in 100 mL toluene is stirred under reflux overnight. The reaction mixture is filtered and concentrated in vacuo. The residue is taken up in ethylacetate and washed with 5% aqueous citric acid, saturated aqueous sodium hydrogencarbonate and brine. The organic phase is dried over MgSO4 and concentrated in vacuo. Yield: 9.37 g.

1. temperatureunder reflux overnight
2. filtrationThe reaction mixture is filtered
3. concentrationconcentrated in vacuo
4. washwashed with 5% aqueous citric acid, saturated aqueous sodium hydrogencarbonate and brine
5. dry with materialThe organic phase is dried over MgSO4
6. concentrationconcentrated in vacuo