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2-Aminopyridine → 2-Amino-1-[3-ethoxy-2,3-dioxo-1-(2-phenylethyl)propyl]pyridinium bromide

HRID 2169006
Notes
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Reaction equation

HRID 2169006 reaction equation
[Br:1][CH:2]([CH2:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:3](=[O:9])[C:4]([O:6][CH2:7][CH3:8])=[O:5].[NH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=1>C1COCC1>[Br-:1].[NH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][N+:20]=1[CH:2]([CH2:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:3](=[O:9])[C:4]([O:6][CH2:7][CH3:8])=[O:5]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 104392-AminopyridineHCID 86642211Ethyl 3-bromo-2-oxo-5-phenylpentanoate

Product 1

HCID 866422092-Amino-1-[3-ethoxy-2,3-dioxo-1-(2-phenylethyl)propyl]pyridinium bromideYield 54.4%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a solution of ethyl 3-bromo-2-oxo-5-phenylpentanoate (1.9 g) in THF (10 ml) was added 2-aminopyridine (600 mg) at room temperature, and the reaction mixture was heated under reflux for 15 hr. The precipitated crystals were collected by filtration, washed with THF to give 2-amino-1-[3-ethoxy-2,3-dioxo-1-(2-phenylethyl)propyl]pyridinium bromide (1.36 g). 2-Amino-1-[3-ethoxy-2,3-dioxo-1-(2-phenylethyl)propyl]pyridinium bromide (1.36 g) was dissolved in ethanol (10 ml), and the mixture was refluxed under heating for 3 hr. The reaction mixture was concentrated, and dissolved in dichloromethane. The solution was washed successively with aqueous sodium bicarbonate and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was recrystallized from ethyl acetate-diethyl ether to give the object product (950 mg).

Workup

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 15 hr
  3. filtrationThe precipitated crystals were collected by filtration
  4. washwashed with THF

Sources & evidence

ORD record
ord-9e0ebb82e3ef41b6911b1e7f7b77deb4
Source dataset
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09045436B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes