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Tetrahydrofuran → 4-(4-Methylenecyclohexyl)-1,3-benzenediol

HRID 585695
Notes
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Reaction equation

HRID 585695 reaction equation
[F-].C([N+](CCCC)(CCCC)CCCC)CCC.C(C[Si]([O:29][C:30]1[CH:35]=[CH:34][CH:33]=[C:32](O[Si](C(C)(C)C)(C)C)[C:31]=1[CH:44]1[CH2:49][CH2:48][C:47](=[CH2:50])[CH2:46][CH2:45]1)(C(C)C)C)(C)(C)C.[O:51]1CCCC1>>[CH2:50]=[C:47]1[CH2:48][CH2:49][CH:44]([C:31]2[CH:32]=[CH:33][C:34]([OH:51])=[CH:35][C:30]=2[OH:29])[CH2:45][CH2:46]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 3

HCID 8028TetrahydrofuranHCID 2724141Tetrabutylammonium Fluoride2×HCID 69780056Tert-butyl-[3-{[tert-butyl(dimethyl)silyl]oxy}-2-(4-methylenecyclohexyl)phenoxy](isopropyl)dimethylsilane

Product 1

HCID 98991634-(4-Methylenecyclohexyl)-1,3-benzenediolYield 90%

Procedure

Tetrabutylammonium fluoride (230 μl) was added to a stirred solution of tert-butyl-[3-{[tert-butyl(dimethyl)silyl]oxy}-2-(4-methylenecyclohexyl)phenoxy](isopropyl)dimethylsilane (40 mg) in tetrahydrofuran (2 ml) at room temperature. After 24 hr, further tetrabutylammonium fluoride (50 μl) was added, and after 2 hr the solvent was removed under reduced pressure. The residue was partitioned between water (20 ml) and ethyl acetate (20 ml). The layers were separated and the aqueous layer was extracted with ethyl acetate (2×20 ml). The combined organic extracts were washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by flash column chromatography (SiO2, ethyl acetate/petrol, 2:3 v/v) to give the title compound as a white solid (17 mg, 90%). δH (CD3OD) 1.25-1.40 (2H, m), 1.75-1.82 (2H, m), 2.04-2.15 (2H, m), 2.22-2.30 (2H, m), 2.86 (1H, tt), 3.20 (1H, m), 4.50 (2H, s), 6.10-6.16 (2H, m), 6.72 (1H, d); m/z (ES+) 205 (M+H)+.

Workup

  1. customafter 2 hr the solvent was removed under reduced pressure
  2. customThe residue was partitioned between water (20 ml) and ethyl acetate (20 ml)
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with ethyl acetate (2×20 ml)
  5. washThe combined organic extracts were washed with brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated in vacuo
  8. customThe residue was purified by flash column chromatography (SiO2, ethyl acetate/petrol, 2:3 v/v)

Sources & evidence

ORD record
ord-ffbdfd15ad194fc6a9abda6ab3248832
Source dataset
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06933319B2

Reaction notes

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