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ChemicalBook CAS DataBase List (3Z)-4-Ethoxy-1,1,1-trifluoro-3-buten-2-one
910136-24-2

(3Z)-4-Ethoxy-1,1,1-trifluoro-3-buten-2-one synthesis

3synthesis methods
-

Yield:910136-24-2 99.5%

Reaction Conditions:

with 4-methyl-morpholine in dichloromethane at 0 - 10; for 1 h;Sealed tube;Reagent/catalyst;Solvent;

Steps:

1-3; 1-4 Example 1

Put 25g of vinyl ether, 100ml of dichloromethane, 38.1g of N-methylmorpholine into a 250ml four-necked bottle, seal the system, cool down to 0-10°C, and start to feed trifluoroacetyl chloride gas into the system through a steel cylinder, The reaction temperature was maintained at 0-10°C.After the aeration volume reaches 45.5g, stop the ventilation, keep the reaction for 1h, and after the sampling analysis is qualified, add 80g of water, stir until the solid is completely dissolved for 10min, then stand for stratification. Sodium sulfate was dried, and the dried organic layer was sampled and detected, and the spectral results were shown in Figure 1.After the solvent was recovered by distillation under reduced pressure, a product with a GC purity of 99% was obtained. The sampling of the product is shown in Figure 2.The yield was 99.5%, and 100% was the cis structure.

References:

CN114956969,2022,A Location in patent:Paragraph 0042-0060