Process for preparing citral
A technology of citral and dehydrolinalool, applied in the preparation of organic compounds, preparation of carbon-based compounds, chemical instruments and methods, etc., can solve the problems of low yield, unsatisfactory and the like, and achieve high reaction yield , The effect of low production cost and simple and convenient post-processing
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Embodiment 1
[0020] With 20.0g (127.8mmol) dehydrolinalool, 4g (51.28mmol) DMSO, 1.0g (3.06mmol) MoO 2 acac 2 And the mixture of 2.0g of weakly acidic cation exchange resin in 100ml of petroleum ether is placed in a 250ml three-necked flask equipped with a thermometer, a stirrer and a condenser. The mixture was then heated to 120°C. During this time, the color of the reaction mixture changed to dark blue or dark green-blue. To control the reaction, gas chromatography (GC) analysis was used. After the reaction was completed, it was cooled to room temperature, and the solid was removed by filtration, then concentrated under reduced pressure and the reaction mixture was worked up by distillation under reduced pressure. The content was determined by GC, and the results are listed in Table 1.
[0021] Table 1
[0022] Reaction time Yield of citral residual dehydrolinalool 4 64.3％ 30.8％ 6 75.0％ 18.3％ 8 84.4％ 6.5％ 10 88.7％ 0％
Embodiment 2
[0024] With 20.0g (127.8mmol) dehydrolinalool, 4g (51.28mmol) DMSO, 2.0g (6.12mmol) MoO 2 acac 2 And the mixture of 4.0g of weakly acidic cation exchange resin in 100ml of petroleum ether is placed in a 250ml three-necked flask equipped with a thermometer, a stirrer and a condenser. The mixture was then heated to 120°C. During this time, the color of the reaction mixture changed to dark blue or dark green-blue. To control the reaction, gas chromatography (GC) analysis was used. After the reaction was completed, it was cooled to room temperature, and the solid was removed by filtration, then concentrated under reduced pressure and the reaction mixture was worked up by distillation under reduced pressure. The content was determined by GC, and the results are listed in Table 2.
[0025] Table 2
[0026] Reaction time Yield of citral residual dehydrolinalool 3 67.2％ 29.7％ 5 78.0％ 16.3％ 7 85.5％ 6.5％ 9 90.2％ 0％
Embodiment 3
[0028] With 20.0g (127.8mmol) dehydrolinalool, 4g (51.28mmol) DMSO, the MoO that embodiment 2 filters recovery 2 acac 2 The mixture of 1.5g (4.59mmol) and 4.0g of weakly acidic cation exchange resin in 100ml of petroleum ether was placed in a 250ml three-necked flask equipped with a thermometer, a stirrer and a condenser. The mixture was then heated to 120°C. During this time, the color of the reaction mixture changed to dark blue or dark green-blue. To control the reaction, gas chromatography (GC) analysis was used. After the reaction was completed, it was cooled to room temperature, and the solid was removed by filtration, then concentrated under reduced pressure and the reaction mixture was worked up by distillation under reduced pressure. The content was determined by GC, and the results are listed in Table 3.
[0029] table 3
[0030] Reaction time Yield of citral residual dehydrolinalool 6 63.1％ 32.6％ 8 73.5％ 21.3％ 10 83.6％ 6.1％ 12...
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