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Sodium hydride → Methyl 5-chloro-2-{[(5-fluoropyridin-3-yl)oxy]methyl}benzoate

HRID 660224
Notes
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Reaction equation

HRID 660224 reaction equation
[F:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([OH:8])[CH:7]=1.[H-].[Na+].Br[CH2:12][C:13]1[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:14]=1[C:15]([O:17][CH3:18])=[O:16]>CN(C)C=O>[Cl:23][C:20]1[CH:21]=[CH:22][C:13]([CH2:12][O:8][C:6]2[CH:5]=[N:4][CH:3]=[C:2]([F:1])[CH:7]=2)=[C:14]([CH:19]=1)[C:15]([O:17][CH3:18])=[O:16]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 24758Sodium hydrideHCID 27629063-Fluoro-5-hydroxypyridineHCID 51358462Methyl 2-(bromomethyl)-5-chlorobenzoate

Product 1

HCID 68865859Methyl 5-chloro-2-{[(5-fluoropyridin-3-yl)oxy]methyl}benzoateYield 53%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent2×

Procedure

To a solution of 3-fluoro-5-hydroxypyridine (34 mg, 0.30 mmol) in dimethylformamide (3 mL) was added sodium hydride (60% dispersion in mineral oil, 12 mg, 0.30 mmol) at 0° C. and the mixture was stirred at room temperature for 15 minutes. To the mixture was added methyl 2-(bromomethyl)-5-chlorobenzoate (100 mg, 0.4 mmol) in dimethylformamide and the mixture was stirred at room temperature overnight. The mixture was quenched with water and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and evaporated. The residue was purified by flash column chromatography on silica gel to afford 47 mg (53%) of the title compound:

Workup

  1. stirringthe mixture was stirred at room temperature overnight
  2. customThe mixture was quenched with water
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customThe residue was purified by flash column chromatography on silica gel

Sources & evidence

ORD record
ord-ad1be1543cdc4254b3cb4c898eb47438
Source dataset
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08084476B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes