Pyridine → HCID 22226281, compound
Reaction equation
[Br:1]C[C:3]1([C:6]([C:8]2(CBr)[CH2:10][CH2:9]2)=[O:7])CC1.[N:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(O)C>[Br-:1].[CH:8]1([C:6]([CH2:3][N+:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:7])[CH2:9][CH2:10]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
2.4 g of 1-bromomethylcyclopropylketone and 5.8 cm3 of pyridine are introduced into a three-necked flask containing 40 cm3 of ethanol and then the mixture is heated for 2 hours under reflux. After concentrating to dryness at 40° C. under reduced pressure (2.7 kPa), the residue is taken up in twice 30 cm3 of diethyl. ether. After filtration, washing with diethyl ether, the precipitate is dried under reduced pressure (90 Pa) to give 3.4 g of 1-cyclopropylcarbonylmethylpyridinium bromide in the form of a cream-coloured solid melting at 160° C.
Workup
- temperaturethe mixture is heated for 2 hours
- temperatureunder reflux
- concentrationAfter concentrating to dryness at 40° C. under reduced pressure (2.7 kPa)
- filtrationAfter filtration
- washwashing with diethyl ether
- customthe precipitate is dried under reduced pressure (90 Pa)
Sources & evidence
- ORD record
- ord-711ededf458c4691a77b233758e28a62
- Source dataset
- uspto-grants-2006_03
- Patent number
- US07019110B2
Reaction notes
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