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Dichloromethane → (4-Bromo-5-methylpyridin-2-yl)methanol

HRID 2080477
Notes
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Reaction equation

HRID 2080477 reaction equation
FC(F)(F)C(O[C:6](=[O:11])[C:7](F)(F)F)=O.ClCCl.[Br:17][C:18]1[C:23]([CH3:24])=[CH:22][N+:21]([O-])=C(C)[CH:19]=1>CCCCCC>[Br:17][C:18]1[C:23]([CH3:24])=[CH:22][N:21]=[C:7]([CH2:6][OH:11])[CH:19]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 9845Trifluoroacetic anhydrideHCID 544438594-Bromo-2,5-dimethylpyridine 1-oxide

Product 1

HCID 23114663(4-Bromo-5-methylpyridin-2-yl)methanolYield 83.3%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

Under an argon atmosphere, trifluoroacetic anhydride (20.6 ml, 0.146 mol) was added to a dichloromethane solution (100 ml) solution of 4-bromo-2,5-dimethylpyridine 1-oxide (9.8 g, 48.5 mmol) under ice cooling. The resulting mixture was stirred for 20 minutes and then, stirred at room temperature for 7.5 hours. The reaction mixture was concentrated under reduced pressure. To a dichloromethane solution (50 ml) of the residue was added a saturated aqueous solution (100 ml) of sodium bicarbonate. The resulting mixture was stirred for 14 hours. The reaction mixture was extracted with dichloromethane. The extract was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography. The fraction obtained from the hexane:ethyl acetate (=1:1) eluate was concentrated under reduced pressure to give the title compound (8.17 g, 40.4 mmol, 83%) as a yellow powder.

Workup

  1. stirringstirred at room temperature for 7.5 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionTo a dichloromethane solution (50 ml) of the residue was added a saturated aqueous solution (100 ml) of sodium bicarbonate
  4. stirringThe resulting mixture was stirred for 14 hours
  5. extractionThe reaction mixture was extracted with dichloromethane
  6. dry with materialThe extract was dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue thus obtained
  9. concentrationethyl acetate (=1:1) eluate was concentrated under reduced pressure

Sources & evidence

ORD record
ord-406bae1fc46848bb8fac4917346b95d2
Source dataset
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07932271B2

Reaction notes

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