4,4-bis(4-fluorophenyl)butan-1-ol synthesis

5synthesis methods

Product Name:4,4-bis(4-fluorophenyl)butan-1-ol
CAS Number:50337-85-4
Molecular formula:C16H16F2O
Molecular Weight:262.3

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50337-85-4
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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