反应详情

To a stirred solution of cyclohexylmethylketone (2.52 g, 20 mmol) in DME (50 mL) at −20° C. was added ethyl difluoroacetate (7.44 g, 60 mmol) and sodium methoxide (6.48 g, 120 mmol), and the resulting reaction mixture was then stirred at room temperature for 1 hour. EtOAc (500 ml) and water (50 ml) were added, and the pH of the aqueous layer was adjusted to 6 by addition of 1 N HCl solution. The organic layer was washed with brine (50 ml), dried over Na2SO4, and concentrated in vacuo to give the title (3.8 g, 93%). This was used for the next coupling step without further purification.

1. customthe resulting reaction mixture
2. washThe organic layer was washed with brine (50 ml)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated in vacuo
5. customto give the title (3.8 g, 93%)
6. customThis was used for the next coupling step without further purification