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ChemicalBook CAS DataBase List 4,4-Difluorocyclohexanecarboxylic acid
122665-97-8

4,4-Difluorocyclohexanecarboxylic acid synthesis

3synthesis methods
-

Yield:122665-97-8 97%

Reaction Conditions:

with water;lithium hydroxide in tetrahydrofuran at 20;

Steps:

12 Example 12
A solution of ethyl 4,4-difluorocyclohexanecarboxylate (0.385 g, 2.003 mmol) in THF (12 mL) was treated with H2O (6 mL) followed by lithium hydroxide monohydrate (0.420 g, 10.02 mmol) and the mixture stirred vigorously at RT overnight.
The mixture was treated with EtOAc, acidified with 1M HCl until pH 4, the layers separated and the aqueous layer extracted with additional EtOAc (1*).
The combined organics were washed with brine, dried over MgSO4 and concentrated to dryness to afford 4,4-difluorocyclohexanecarboxylic acid (318 mg, 97%) as a white solid. 1H NMR (400 MHz, DMSO-d6): δ 12.28 (s, 1H), 2.40 (m, 1H), 2.02-1.75 (m, 6H), 1.59 (m, 2H).

References:

Deciphera Pharmaceuticals, LLC;Flynn, Daniel L.;Caldwell, Timothy Malcolm;Kaufman, Michael D.;Patt, William C.;Samarakoon, Thiwanka;Vogeti, Lakshminarayana;Yates, Karen M. US2014/275080, 2014, A1 Location in patent:Paragraph 0428

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