The preparation method of 1-(2,6,6-trimethyl-cyclohexenyl)-2-butene-1-one
A technology of cyclohexenyl and trimethyl, applied in the field of preparation of 1--2-buten-1-one, can solve the problem of high price
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[0033] The invention provides a preparation method of 1-(2,6,6-trimethyl-cyclohexenyl)-2-buten-1-one, comprising the following steps:
[0034] Isomerizing 1-(2,6,6-trimethyl-3-cyclohexenyl)-1,3-butanedione to obtain an isomerized product;
[0035] reacting the isomerized product to obtain 1-(2,6,6-trimethyl-cyclohexenyl)-2-buten-1-one;
[0036] The 1-(2,6,6-trimethyl-cyclohexenyl)-2-buten-1-one includes 1-(2,6,6-trimethyl-cyclohex-1-ene- yl)-2-buten-1-one and 1-(2,6,6-trimethyl-cyclohex-2-en-yl)-2-buten-1-one.
[0037] Compared with the prior art, the present invention avoids the step of oxidizing alcohols into ketones, and causes less pollution to the environment; the present invention uses 1-(2,6,6-trimethyl-3-cyclohexenyl) -1,3-Butanedione as a raw material can simultaneously obtain 1-(2,6,6-trimethyl-cyclohex-1-enyl)-2-buten-1-one and 1-(2, 6,6-trimethyl-cyclohex-2-enyl)-2-buten-1-one, the preparation method is simple, easy to realize large-scale production; 1-(2,6,6- ...
Embodiment 1
[0084] Add 300mL xylene and 46.8g (1.2mol) sodium amide to the reaction flask, adjust the temperature to 50°C, and add 166g (1.0mol) 1-(2,6,6-trimethylcyclohexyl-3- Alkenyl) ethyl ketone, the temperature is controlled at 50°C, and the drop is completed in about 2 hours. After the dropwise addition, continue to react at a constant temperature of 50°C for 0.5 hours, the reaction solution is cooled to 30°C, and 184g (1.8mol) of acetic anhydride is slowly added dropwise, and the reaction The temperature was controlled at 30°C, the dropwise addition was completed in about 2 hours, and the constant temperature reaction was continued for 1 hour.
[0085] Slowly add 500mL of water to the obtained reaction solution, stir completely and then separate into layers, then add 300mL of 10% sulfuric acid, stir completely and then separate into layers, neutralize the oil layer with 3% sodium hydroxide solution to neutrality, then add 300mL of water to wash; The solvent was recovered, rectified...
Embodiment 2
[0128] In the reaction flask, add 600mL DMF, 96g (1.0mol) sodium tert-butoxide, 180g (0.86mol) 1-(2,6,6-trimethyl-3-cyclohexenyl)-1 prepared in Example 1 , 3-butanedione, stirred at 30°C for 3 hours, the reaction solution was cooled to room temperature, poured into 605g of 10% acetic acid solution, stirred for 10 minutes, then left to separate the liquids, washed the organic layer with water, rectified, and collected 98- 99°C / 2mmHg and 104~105°C / 2mmHg fractions, 58g of intermediate 2a (content 95.8%) and 88g of intermediate 2b (content 95.1%) were obtained, with a yield of 81.1%.
[0129] After analysis, it can be seen that the 2a is 1-(2,6,6-trimethyl-2-cyclohexenyl)-1,3-butanedione, and 2b is 1-(2,6,6-trimethyl -1-cyclohexenyl)-1,3-butanedione.
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