Pyridinium chloride → HCID 15334439, compound
Reaction equation
[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([C:18]#[N:19])=[C:14]([O:20]C)[CH:13]=2)=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.Cl.N1C=CC=CC=1>O>[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([C:18]#[N:19])=[C:14]([OH:20])[CH:13]=2)=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:9])[F:10])[CH:7]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
5.0 g of 3-chloro-2-(4-cyano-3-methoxyphenyl)-5-trifluoromethylpyridine and 5.5 g of pyridine hydrochloride were stirred for 2 hours at 200° C. After cooling, the reaction mixture was thoroughly stirred with 100 ml of water. The solid portion was then separated off and purified by means of column chromatography on silica gel (cyclohexane/methyl tert-butyl ether (2:1) as eluent). Yield: 3.4 g (71%) of white crystals having a melting point of 155°-157° C.
Workup
- temperatureAfter cooling
- customThe solid portion was then separated off
- custompurified by means of column chromatography on silica gel (cyclohexane/methyl tert-butyl ether (2:1) as eluent)
Sources & evidence
- ORD record
- ord-a9704b77a9ca4095a3855130e14e6d66
- Source dataset
- uspto-grants-1998_05
- Patent number
- US05747422
Reaction notes
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