ETHYL 2-METHYL-4,4,4-TRIFLUOROACETOACETATE synthesis
- Product Name:ETHYL 2-METHYL-4,4,4-TRIFLUOROACETOACETATE
- CAS Number:344-00-3
- Molecular formula:C7H9F3O3
- Molecular Weight:198.14
383-63-1
497 suppliers
$10.00/25 g
105-37-3
408 suppliers
$10.00/5mL
344-00-3
117 suppliers
$13.00/1g
Yield:344-00-3 60 g
Reaction Conditions:
with sodium hydride in tetrahydrofuran;mineral oil at 50; for 16 h;
Steps:
To a solution of ethyl propionate (35.0 g, 340 mmol) in THF (350 mL) at 25° C. was added sodium hydride (60% in mineral oil, 13.7 g, 343 mmol). The grey slurry was heated to 50° C. and ethyl trifluoroacetate (97.4 g, 685 mmol) was added dropwise to the mixture over 15 min. The reaction was stirred at 50° C. for 16 h. The cooled reaction mixture was slowly added to 10% sulfuric acid at 0° C. The resulting yellow mixture was extracted with EtOAc (3×500 mL) and the combined organic layers were dried over Na2SO4, filtered and concentrated to give ethyl 4,4,4-trifluoro-2-methyl-3-oxobutanoate (60 g) which was used directly in the next step.
References:
Pfizer Inc.;Dowling, Matthew;Fernando, Dilinie;Futatsugi, Kentaro;Huard, Kim;Magee, Thomas Victor;Raymer, Brian;Shavnya, Andre;Smith, Aaron;Thuma, Benjamin;Tsai, Andy;Tu, Meihua US2017/183328, 2017, A1 Location in patent:Paragraph 0258
383-63-1
497 suppliers
$10.00/25 g
344-00-3
117 suppliers
$13.00/1g
