Thiophosgene → 4-Cyano-2,5-difluoro-phenyl isothiocyanate
Reaction equation
[C:1]([C:3]1[C:9]([F:10])=[CH:8][C:6]([NH2:7])=[C:5]([F:11])[CH:4]=1)#[N:2].[C:12](Cl)(Cl)=[S:13]>C1(C)C=CC=CC=1>[C:1]([C:3]1[C:9]([F:10])=[CH:8][C:6]([N:7]=[C:12]=[S:13])=[C:5]([F:11])[CH:4]=1)#[N:2]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
10.0 g (65 mmol) of 4-cyano-2,5-difluoro-aniline are introduced into 100 ml of toluene and 8.2 g (71 mmol) of thiophosgene are slowly added to the mixture heated to 80° C. to 90° C. The reaction mixture is then refluxed for approximately 40 hours. Then, after the solvent has been carefully distilled off under reduced pressure, the product (4-cyano-2,5-difluoro-phenyl isothiocyanate) is obtained as an ochre colourant.
Workup
- additionare slowly added to the mixture
- temperatureheated to 80° C. to 90° C
- temperatureThe reaction mixture is then refluxed for approximately 40 hours
- distillationThen, after the solvent has been carefully distilled off under reduced pressure
Sources & evidence
- ORD record
- ord-ccbe2fe6b47046218ece3ff2a8b4e13e
- Source dataset
- uspto-grants-2002_01
- Patent number
- US06339044B1
Reaction notes
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