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Methanol → (3-Bromo-5-fluorophenyl)methanol

HRID 595981
Notes
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Reaction equation

HRID 595981 reaction equation
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([F:11])[CH:10]=1)[C:5](O)=[O:6].B.C1COCC1.CO>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([CH2:5][OH:6])[CH:8]=[C:9]([F:11])[CH:10]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 887MethanolHCID 2723981Borane;tetrahydrofuranHCID 27733393-Bromo-5-fluorobenzoic acid

Product 1

HCID 2769402(3-Bromo-5-fluorophenyl)methanol

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a suspension of 3-bromo-5-fluorobenzoic acid (4.51 g, 20.59 mmol) in THF (41.2 mL) at 0° C., BH3.THF (41.2 mL, 41.2 mmol) was added dropwise over 30 min, the reaction mixture was then allowed to return to room temperature and stirred at room temperature overnight. Methanol (40 mL) was added slowly and stirred at room temperature for 1 h. THF and Methanol was removed in vacuo. The residue was then extracted by EtOAc, and washed with sat.NaHCO3, The organic was dried and concentrated. The crude product was used in next step reaction without purification. LCMS (m/z): 187.2 (MH+−18), 0.66 min. 1H NMR (400 MHz, CDCl3) δ ppm 7.32 (s, 1H), 7.19-7.14 (m, 1H), 7.05 (tdd, J=0.7, 1.5, 9.1 Hz, 1H), 4.70 (br. s., 2H), 1.78 (br. s., 1H).

Workup

  1. customto return to room temperature
  2. stirringstirred at room temperature for 1 h
  3. customTHF and Methanol was removed in vacuo
  4. extractionThe residue was then extracted by EtOAc
  5. washwashed
  6. dry with materialNaHCO3, The organic was dried
  7. concentrationconcentrated
  8. customThe crude product was used in next step reaction without purification
  9. custom187.2 (MH+−18), 0.66 min

Sources & evidence

ORD record
ord-ce263cb54f1843f780e6e27dc29f5c26
Source dataset
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09242996B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes