反应详情

Sodium azide (1.05 g, 16.2 mmol) and lithium perchlorate (6.45 g, 60.7 mmol) are added to a solution of 5-(oxiran-2-yl)-2-(2,2,2-trifluoroethoxy)pyridine (0.89 g, 4.04 mmol, Step-5, single enantiomer) in acetonitrile (100 mL) is refluxed with stirring for 5 hours. White precipitate is filtrated and filtrate is concentrated in vacuo. The residue is poured into water, extracted with ethyl acetate and dried over sodium sulfate and concentrated in vacuo. The residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (1:1) to give 0.39 g (37% yield) of the title compound as colorless oil.

1. temperatureis refluxed
2. filtrationWhite precipitate is filtrated
3. concentrationfiltrate is concentrated in vacuo
4. additionThe residue is poured into water
5. extractionextracted with ethyl acetate
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated in vacuo
8. customThe residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (1:1)