2,4,5-TRIMETHOXYLPRORIOPHENONE synthesis
- Product Name:2,4,5-TRIMETHOXYLPRORIOPHENONE
- CAS Number:3904-18-5
- Molecular formula:C12H16O4
- Molecular Weight:224.25
with propionic anhydride catalyzed either by iodine or aluminium chloride;
with propionyl chloride in the presence of aluminium chloride in methylene chloride at 10° for 1 h (80%)or in carbon disulfide (67%).
Yield:3904-18-5 96%
Reaction Conditions:
with aluminum (III) chloride in dichloromethane at 5 - 20; for 1.5 h;Large scale;
Steps:
1.1; 2.1 1. Preparation of 2,4,5-trimethoxy-1-phenyl ethyl ketone
10 kg of 1,2,4-trimethoxybenzene, 6.5 kg of propionyl chloride, 55 kg of dichloromethane were put into the reaction kettle, stirred and cooled to 5 ° C, and 9 kg of aluminum trichloride was added in 4 portions.Each time aluminum trichloride was added to keep the temperature below 20 ° C, the reaction was stirred at room temperature for 1.5 hours.After the concentration of the reaction product was stabilized by TLC, the mixture was discharged to 40 kg of ice, and the oil and water layers were separated by stirring, and the oil layer was washed once with 20 liters of water. Combine the washing liquid and the water layer,Extract twice with 10 liters of dichloromethane, then wash the resulting extract once with 10 liters of water.The washed extract and the oil phase after washing are combined.Dry with 2.5 kg of sodium hydroxide for 1 hour, add 2.5 kg of anhydrous sodium sulfate, filter out the solid,Evaporate the dichloromethane in a water bath (recovery of 64 kg of dichloromethane), and crystallize at room temperature.The product obtained by filtration was 12.8 kg, and the yield was 96%.
References:
CN110128248,2019,A Location in patent:Paragraph 0044-0047; 0054-0057
6906-65-6
0 suppliers
inquiry
3904-18-5
10 suppliers
inquiry
29652-82-2
0 suppliers
inquiry
3904-18-5
10 suppliers
inquiry