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Methylamine → 4-Chloro-5-fluoro-2-(N-methylaminomethyl)-pyridine

HRID 1866
Notes
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Reaction equation

HRID 1866 reaction equation
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][NH:5][C:4](Br)([CH3:9])[CH:3]=1.[CH3:11][NH2:12]>CO>[Cl:1][C:2]1[C:7]([F:8])=[CH:6][N:5]=[C:4]([CH2:9][NH:12][CH3:11])[CH:3]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 6329MethylamineHCID 867500424-Chloro-5-fluoro-alpha-bromo-2-picoline

Product 1

HCID 196914964-Chloro-5-fluoro-2-(N-methylaminomethyl)-pyridineYield 70%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

4-Chloro-5-fluoro-alpha-bromo-2-picoline (1.37 g, 6.1 mmol), from Step 1 was dissolved in 15 mL of methanol in a pressure tube. Methylamine (3 mL of 40% aqueous solution) was added to the tube and the tube was sealed. The reaction mixture was stirred at ambient temperature for 26 hours and then the solvent was removed under reduced pressure. To the residue was added 50 mL of 10% aqueous sodium carbonate solution and the resultant aqueous mixture was extracted with 3 X 50 mL of methylene chloride. The organic combined extract was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressur. The residue was dried in vacuo to give 754 mg g (70% yield) of the title compound; MS DCI-NH3M/Z: 175 (M+H)+ base; 1H NMR (CDCl3) d 2.50 (s, 3H), 3.90 (s, 2H), 7.47 (d, 1H), 8.42 (s, 1H).

Workup

  1. customthe tube was sealed
  2. customthe solvent was removed under reduced pressure
  3. additionTo the residue was added 50 mL of 10% aqueous sodium carbonate solution
  4. extractionthe resultant aqueous mixture was extracted with 3 X 50 mL of methylene chloride
  5. extractionThe organic combined extract
  6. dry with materialwas dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressur
  9. customThe residue was dried in vacuo

Sources & evidence

ORD record
ord-a310f335f3e844efadd43206c4a310e4
Source dataset
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05726182

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes