反应详情

Tosyl chloride (0.0814 mol) was added to a cooled (0°) solution of 3-(3,5-difluorophenyl)propanol (0.0407 mol) in pyridine (75 ml). The reaction was stirred 2 hours at 25°, then it was poured into ice/water and extracted into ethyl ether. The ethereal extracts were washed with 3N aqueous hydrogen chloride and water, then were dried over sodium sulfate and concentrated. The residue was dissolved in dimethylformamide (75 ml) and sodium azide (0.0814 mol) was added. The reaction was stirred 8 hours, then was diluted with water and extracted into ethyl acetate. The organic extract was washed with 3N aqueous hydrogen chloride and water, then dried over sodium sulfate and concentrated to yield 6.7 g (64%) of an oily product.

1. extractionextracted into ethyl ether
2. washThe ethereal extracts were washed with 3N aqueous hydrogen chloride and water
3. dry with materialwere dried over sodium sulfate
4. concentrationconcentrated
5. dissolutionThe residue was dissolved in dimethylformamide (75 ml)
6. stirringThe reaction was stirred 8 hours
7. extractionextracted into ethyl acetate
8. extractionThe organic extract
9. washwas washed with 3N aqueous hydrogen chloride and water
10. dry with materialdried over sodium sulfate
11. concentrationconcentrated