Preparation method of industrial musk tonalide
An industrial technology of musk tona, which is applied in the direction of condensation preparation of carbonyl compounds, organic chemistry, etc., can solve the problems of human skin damage, rising demand and high production cost, and achieves the effects of low production cost, mild conditions and high yield.
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Embodiment 1
[0023] Step 1, preparation of intermediate 1,1,3,4,4,6-hexamethyltetralin
[0024] 1) Take 2 moles of p-cymene, 1 mole of 2,3-dimethyl-1-butene and 1.05 moles of tert-butyl chloride according to the molecular mass ratio, and mix them to form the material reaction solution A-1 ,spare;
[0025] 2) At 20°C, take 10 parts of anhydrous aluminum trichloride, 1 part of concentrated sulfuric acid, 0.5 parts of hydrochloric acid, and 2 parts of cyclohexane according to the ratio of parts by weight, and first mix the concentrated sulfuric acid, hydrochloric acid and cyclohexane , and then add anhydrous aluminum trichloride while stirring to form a reaction mixture A-2 after the reaction is terminated, for subsequent use;
[0026] 3) According to the ratio of parts by weight, take 1 part of the material reaction solution A-1 and gradually add it dropwise to 1.2 parts of the reaction mixture A-2. The dropping time is 50 minutes. After the dropping is completed, use thin-layer chromatogra...
Embodiment 2
[0036] Step 1, preparation of intermediate 1,1,3,4,4,6-hexamethyltetralin
[0037] 1) Take 2.5 moles of p-cymene, 1.25 moles of 2,3-dimethyl-1-butene and 1.25 moles of tert-butyl chloride according to the molar mass ratio, and mix them to form the material reaction solution A-1 ,spare;
[0038] 2) At 23°C, take 10 parts of anhydrous aluminum trichloride, 1 part of concentrated sulfuric acid, 0.5 parts of hydrochloric acid, and 3 parts of cyclohexane according to the ratio of parts by weight, and first mix the concentrated sulfuric acid, hydrochloric acid and cyclohexane , and then add anhydrous aluminum trichloride while stirring to form a reaction mixture A-2 after the reaction is terminated, for subsequent use;
[0039] 3) According to the ratio of parts by weight, take 1 part of the material reaction solution A-1 and gradually add it dropwise to 1.3 parts of the reaction mixture A-2. The dropping time is 60 minutes. After the dropping is completed, use thin-layer chromatog...
Embodiment 3
[0049] Step 1, preparation of intermediate 1,1,3,4,4,6-hexamethyltetralin
[0050] 1) Take 3 moles of p-cymene, 1.5 moles of 2,3-dimethyl-1-butene and 1.40 moles of tert-butyl chloride according to the molar mass ratio, and mix them to form the material reaction solution A-1 ,spare;
[0051] 2) At 25°C, take 10 parts of anhydrous aluminum trichloride, 1 part of concentrated sulfuric acid, 0.5 parts of hydrochloric acid, and 4 parts of cyclohexane according to the ratio of parts by weight, and first mix the concentrated sulfuric acid, hydrochloric acid and cyclohexane , and then add anhydrous aluminum trichloride while stirring to form a reaction mixture A-2 after the reaction is terminated, for subsequent use;
[0052] 3) According to the ratio of parts by weight, take 1 part of the material reaction solution A-1 and gradually add it dropwise to 1.5 parts of the reaction mixture A-2. The dropping time is 70 minutes. After the dropping is completed, use thin-layer chromatograp...
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