反应详情

A solution of 3.6 g. of 2-acetyl-5 -methylcyclohexanone and 5.6 g. of 5-(1,2-dimethylheptyl)resorcinol in 150 ml. of acetic acid is cooled to 15° and saturated with hydrogen chloride gas. The solution is allowed to warm to 25°, stirred for 20 hours and then heated for one hour on a steam bath. The reaction mixture is concentrated in vacuo, water is added and the residue is dissolved in ethyl acetate. The ethyl acetate solution is washed with water, dried (MgSO4) and concentrated to give a residue which is distilled five times, b.p. 195°-200° (0.025 mm.). The distillate is chromatographed on silica gel with benzene as eluant. The second fraction is collected and distilled to give the title compound, b.p. 190°-195° (0.05 mm.).

1. temperatureto warm to 25°
2. temperatureheated for one hour on a steam bath
3. concentrationThe reaction mixture is concentrated in vacuo, water
4. additionis added
5. dissolutionthe residue is dissolved in ethyl acetate
6. washThe ethyl acetate solution is washed with water
7. dry with materialdried (MgSO4)
8. concentrationconcentrated
9. customto give a residue which
10. distillationis distilled five times, b.p. 195°-200° (0.025 mm.)
11. distillationThe distillate is chromatographed on silica gel with benzene as eluant
12. customThe second fraction is collected
13. distillationdistilled