Dichloromethane → HCID 22617181, compound
Reaction equation
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[NH:13][C:14](=O)[C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cl:42]CCl>C(Cl)(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[N:13]=[C:14]([Cl:42])[C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
First, 4.3 g (11 mmol) of N-(2,6-dichloro-4-trifluoromethylphenyl)-2,2,3,3,3-pentafluoropropionamide was dissolved in 22 ml of dichloromethane, to which 1.8 ml of carbon tetrachloride and 4.5 g (17 mmol) of triphenylphosphine were added at room temperature, and the mixture was stirred for 18 hours. The reaction mixture was concentrated under reduced pressure, followed by addition of hexane, and undissolved matter was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 3.8 g of N-(2,6-dichloro-4-trifluoromethylphenyl)-2,2,3,3,3-pentafluoropropionimidoyl chloride.
Workup
- additionwere added at room temperature
- concentrationThe reaction mixture was concentrated under reduced pressure
- additionfollowed by addition of hexane, and undissolved matter
- customwas removed by filtration
- concentrationthe filtrate was concentrated under reduced pressure
Sources & evidence
- ORD record
- ord-d04ddabd37454f45afeeafed5cc88208
- Source dataset
- uspto-grants-2002_04
- Patent number
- US06376710B2
Reaction notes
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