Ethanone, 2,2-difluoro-2-iodo-1-phenyl- synthesis
- Product Name:Ethanone, 2,2-difluoro-2-iodo-1-phenyl-
- CAS Number:150542-06-6
- Molecular formula:C8H5F2IO
- Molecular Weight:282.03
1259998-89-4
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Yield:150542-06-6 60%
Reaction Conditions:
Stage #1: 2,2,4,4,4-pentafluoro-3,3-dihydroxy-1-phenylbutan-1-onewith iodine;lithium bromide in tetrahydrofuran; for 0.166667 h;
Stage #2: with triethylamine in tetrahydrofuran at 20; for 0.5 h;
Steps:
1.3 Synthesis of Fluoride Block IV:
Add the crude product III to a dry 250mL round bottom flask, add dry tetrahydrofuran, stir until fully dissolved, add anhydrous lithium bromide (256mmol, 22.2g, 6equiv), stir well, and then add iodine element (80mmol, 20.3g) , 2equiv), continue to stir for 10min, and then add triethylamine (80mmol, 8g, 2equiv) dropwise. After the addition is complete, stir the reaction at room temperature for 30min. Follow the detection with a chromatography plate until the reaction is complete. After quenching, extraction, washing, drying and filtering, the filtrate was spin-dried on a rotary evaporator to obtain the crude product IV. The column was separated by column chromatography with a volume ratio of petroleum ether: ethyl acetate = 100: 1. Finally, a bright yellow oily liquid (yield 60%) is obtained, which is a fluorine-containing building block IV.
References:
CN110627628,2019,A Location in patent:Paragraph 0035; 0036; 0042-0045
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