反应详情

Jones reagent (e.g. an aqueous sulfuric acid solution of chromium trioxide) was added to a solution of 3-chloro-4,5-dipropargyloxybenzaldehyde (18.0 g) in acetone (100 ml) under stirring at a temperature below 20° C. The addition was stopped when the reaction mixture became red, and stirring was continued at 20° C. for 1 hour. The reaction mixture was poured into ice-water containing ethanol (100 nl) and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate and concentrated under reduced pressure. The residue was washed with hexane to give 3-chloro-4,5-dipropargyloxybenzoic acid (16.2 g). m.p. 158°-159° C.

1. additionThe addition
2. stirringstirring
3. extractionextracted with ethyl acetate
4. washThe extract was washed with water
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. washThe residue was washed with hexane