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Dimethylformamide → 4-Chloro-5-fluoropyridine-3-carbaldehyde

HRID 715932
Notes
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Reaction equation

HRID 715932 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[F:8].C([N-]C(C)C)(C)C.[Li+].CN(C)[CH:19]=[O:20]>O1CCCC1>[Cl:1][C:2]1[C:3]([F:8])=[CH:4][N:5]=[CH:6][C:7]=1[CH:19]=[O:20]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 6228DimethylformamideHCID 2724682Lithium diisopropylamideHCID 38524294-Chloro-3-fluoropyridine

Product 1

HCID 717423064-Chloro-5-fluoropyridine-3-carbaldehyde

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Conditions

Temperature
-78 °C

Procedure

4-Chloro-3-fluoropyridine (1 g) was dissolved in tetrahydrofuran (15 ml), and the solution was then cooled to −78° C. Lithium diisopropylamide (1.1 M solution in tetrahydrofuran and n-hexane, 7.6 ml) was added dropwise thereto, and the mixture was stirred at the same temperature as above for 5 hours. Then, N,N-dimethylformamide (1 ml) was added thereto, and the mixture was further stirred for 30 minutes while being heated to room temperature. Saturated saline was added to the reaction solution, followed by extraction with ethyl acetate. The extract was washed with water and saturated saline in this order and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel chromatography (n-hexane-ethyl acetate) to obtain the title compound (521 mg).

Workup

  1. stirringthe mixture was further stirred for 30 minutes
  2. temperaturewhile being heated to room temperature
  3. additionSaturated saline was added to the reaction solution
  4. extractionfollowed by extraction with ethyl acetate
  5. washThe extract was washed with water and saturated saline in this order
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled off under reduced pressure
  8. customThe obtained residue was purified by silica gel chromatography (n-hexane-ethyl acetate)

Sources & evidence

ORD record
ord-b04ae81d28414ccd935165ee28c34685
Source dataset
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09187489B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes