4,4-bis(4-fluorophenyl)butan-1-ol synthesis
- Product Name:4,4-bis(4-fluorophenyl)butan-1-ol
- CAS Number:50337-85-4
- Molecular formula:C16H16F2O
- Molecular Weight:262.3
20662-52-6
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Yield:50337-85-4 92.6%
Reaction Conditions:
Stage #1: 4,4-bis(4-fluorophenyl)butanoic acidwith lithium aluminium tetrahydride;potassium carbonate in 2-methyltetrahydrofuran at 0 - 10;
Stage #2: with water;sodium hydroxide in 2-methyltetrahydrofuran at 10;Reagent/catalyst;Solvent;Temperature;
Steps:
1.1; 2.1 (1) Synthesis of intermediate I
Put 4,4-bis(4-fluorophenyl)butyric acid 20g (0.072mol) in a three-necked flask,172g (2.00 mol) of methyltetrahydrofuran was stirred and dissolved,Add 5.4g (0.039mol) of potassium carbonate, control the temperature below 10, slowly add 2.89g (0.076mol) of lithium aluminum hydride, keep at 0-10 and stir for 1-2h. After the reaction,When the temperature is controlled below 10°C, 2.9g (0.161mol) of water is added dropwise,15% sodium hydroxide solution (mass fraction) 2.9g (0.011mole),Water 8.7g (0.483mole), after quenching, naturally heated to 25-30, filtered,The filter cake was washed with methyltetrahydrofuran, and the combined filtrate was concentrated to dryness.The product 4,4-bis(4-fluorophenyl)-1-butanol 17.5g (yield 92.6%) was obtained.
References:
CN111196781,2020,A Location in patent:Paragraph 0048-0052; 0061-0063
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