PSEUDOIONONE synthesis
- Product Name:PSEUDOIONONE
- CAS Number:141-10-6
- Molecular formula:C13H20O
- Molecular Weight:192.3
Yield:141-10-6 96.85%
Reaction Conditions:
with sodium acetate;sodium hydroxide in water at 5 - 90;Reagent/catalyst;Temperature;
Steps:
1-4; 1-5 Example 1
1) Continuously mix citral (97% by mass) and acetone at a molar ratio of 1:15, and dissolve sodium hydroxide and sodium acetate with a mass ratio of 4:1 in water to prepare a mass concentration of 1% alkali solution. The mixed citral-acetone solution is introduced into the pipeline reactor (inner diameter φ is 3mm, total length L is 1500mm, stainless steel (304) pipeline) at a flow rate of 12mL/min and alkali solution at a flow rate of 4mL/min. The pipeline reactor includes reaction section I, reaction section II and reaction section III of equal length in sequence along the flow direction. The external temperature of reaction section I is 5, the external temperature of reaction section II is 15, and the external temperature of reaction section III is 85°C. (2) The reaction liquid flowing out of the pipeline reactor enters the triple reactor for the recovery of unreacted acetone. The external temperature of the first reactor is 86 °C, the external temperature of the second reactor is 88 °C and the third reactor the external temperature of 90 °C; The solvent volume recovered in the first reactor is 80% of the total recovered volume, and the volume ratio of acetone to water is 96:4; The amount of solvent recovered in the second reactor is 15% of the total recovered volume, and the volume ratio of acetone to water is 92:8; the volume of solvent recovered in the third reactor is 5% of the total recovered volume, and the volume ratio of acetone to water is 89:11. (3) The deacetone product flowing out of the triple reactor enters the extraction device, and the dichloromethane extractant is added for extraction and stratification. The obtained pseudoionone crude oil is neutralized to a pH value with an acetic acid aqueous solution with a mass concentration of 5% about 7. When the injection volume of citral is 15.2g, the final crude oil of pseudoionone is 19.5g, the content of pseudoionone is 92.5%, the conversion rate of citral is 99.8%, and the yield of pseudoionone is 96.85%. The total recovered acetone was 110 mL, the acetone content of the recovered solvent was 95.1%, and the water content of the recovered solvent was 4.8%. After extraction and separation, the volume of the water layer is 38.5mL, and the alkali content is 1%.
References:
CN112638855,2021,A Location in patent:Paragraph 0035-0084
106-24-1
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141-10-6
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