反应详情

温度

50 °C

A solution of chromium trioxide (55.5 g, 0.555 mol) in water (68 ml) and 2M-sulphuric acid (12 ml) was added dropwise to a solution of 3,7-dimethyloctanol (43.7 g, 0.308 mol) in acetone (100 ml), the temperature was maintained at 40-60° C. and the reaction mixture was left stirring overnight. Acetone was carefully removed in vacuo, the reaction mixture was diluted in water and washed with diethyl ether (2×200 ml). The ethereal solution was washed with 10% sodium hydroxyde solution (200 ml); and the aqueous phase was acidified with 36% HCl (200 ml) and washed once more with diethyl ether (2×200 ml). The organic layer was dried (MgSO4) and the diethyl ether was removed in vacuo. The crude product was distilled to give a colourless oil.

1. waitthe reaction mixture was left
2. customAcetone was carefully removed in vacuo
3. additionthe reaction mixture was diluted in water
4. washwashed with diethyl ether (2×200 ml)
5. washThe ethereal solution was washed with 10% sodium hydroxyde solution (200 ml)
6. washwashed once more with diethyl ether (2×200 ml)
7. dry with materialThe organic layer was dried (MgSO4)
8. customthe diethyl ether was removed in vacuo
9. distillationThe crude product was distilled
10. customto give a colourless oil