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Dichloromethane → 5-Benzyloxy-2-but-1-enylphenol

HRID 398181
Notes
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Reaction equation

HRID 398181 reaction equation
[Br-].[CH2:2]([P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH2:3][CH3:4].C([Li])CCC.[CH2:29]([O:36][C:37]1[CH:44]=[CH:43][C:40]([CH:41]=O)=[C:39]([OH:45])[CH:38]=1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.ClCCl>C1COCC1>[CH2:29]([O:36][C:37]1[CH:44]=[CH:43][C:40]([CH:41]=[CH:2][CH2:3][CH3:4])=[C:39]([OH:45])[CH:38]=1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 6344DichloromethaneHCID 80374Propyltriphenylphosphonium bromideHCID 5612354-Benzyloxy-2-hydroxybenzaldehydeHCID 178418339Butyllithium

Product 1

HCID 693132605-Benzyloxy-2-but-1-enylphenolYield 90%

Reagents, catalysts & solvents 1

HCID 8028
Tetrahydrofuran
Solvent

Procedure

To a flame dried 500 mL 3-neck flask under an atmosphere of argon, was charged n-propyltriphenylphosphonium bromide (12.66 g, 32.85 mmol) dissolved in anhydrous THF (85 mL), followed by the dropwise addition of n-butyllithium 16.4 mL, 26.28 mmol). The dark red mixture was stirred at ambient temperature for 1 h. 15 min. Next 4-benzyloxy-2-hydroxybenzaldehyde (1.5 g, 6.57 mmol) (Synth. Commun., 26(3), 593-601, (1996) was added followed by the addition of anhydrous dichloromethane (27 mL). The mixture was stirred at ambient temperature for 18 h. The solvents were removed in vacuo, and the residue was partitioned between ethyl acetate and water (500 mL each). The organic layer was washed with brine (500 mL), dried (Na2SO4), and concentrated in vacuo. The crude product was purified using the Biotage FlashElute chromatography system using a 65M normal phase cartridge, eluting with 15% ethyl acetate/Hex to give a yellow solid (1.50 g, 90%). 1H NMR (400 MHz, CDCl3) δ7.43-7.30 (m, 5H), 7.19 (d, J=8.3 Hz, 1H), 6.52 (dd, J=8.8, 2.4 Hz, 1H), 6.46 (d, J=2.4 Hz, 1H), 6.43 (s, 1H), 6.14-6.07 (m, 1H), 5.03 (s, 2H), 4.98 (s, 1H), 2.25 (quintet, J=7.6 Hz, 2H), 1.09 (t, J=7.3 Hz, 3H), MS (ES) m/e 255 (M+1).

Workup

  1. customTo a flame dried 500 mL 3-neck flask under an atmosphere of argon
  2. custom15 min
  3. addition, 26(3), 593-601, (1996) was added
  4. stirringThe mixture was stirred at ambient temperature for 18 h
  5. customThe solvents were removed in vacuo
  6. customthe residue was partitioned between ethyl acetate and water (500 mL each)
  7. washThe organic layer was washed with brine (500 mL)
  8. dry with materialdried (Na2SO4)
  9. concentrationconcentrated in vacuo
  10. customThe crude product was purified
  11. washeluting with 15% ethyl acetate/Hex

Sources & evidence

ORD record
ord-6eeb56172a45451088e4bff61b0f4d27
Source dataset
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06610696B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes