反应详情

A solution of n-butyllithium (10.0M in hexane; 25.0 ml, 0.25 mol) was added dropwise to a stirred, cooled (-78° C.) solution of 3,5-difluoroanisole (35.9 g, 0.25 mol) in dry THF (200 ml) under dry nitrogen. The stirred mixture was maintained under these conditions for 2.5 h and then poured into a slurry of solid carbon dioxide and dry ether. The product was extracted into 10% sodium hydroxide (twice), the combined basic extracts were acidified with 36% hydrochloric acid, and the product was extracted into ether (twice), the combined ethereal extracts were washed with water and dried (MgSO4). The solvent was removed in vacuo to give a colourless solid.

1. temperatureThe stirred mixture was maintained under these conditions for 2.5 h
2. extractionThe product was extracted into 10% sodium hydroxide (twice), the combined basic extracts
3. extractionthe product was extracted into ether (twice), the combined ethereal extracts
4. washwere washed with water
5. dry with materialdried (MgSO4)
6. customThe solvent was removed in vacuo
7. customto give a colourless solid