Dichloromethane → Trifluoromethyl 1-chloro-N-(p-chlorobenzyl)thioformimidate

HRID 129646Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 129646
[F:1][C:2]([F:6])([F:5])[S:3]Cl.[Cl:7][C:8]1[CH:16]=[CH:15][C:11]([CH2:12][N+:13]#[C-:14])=[CH:10][CH:9]=1.C(Cl)[Cl:18]>>[Cl:18][C:14](=[N:13][CH2:12][C:11]1[CH:15]=[CH:16][C:8]([Cl:7])=[CH:9][CH:10]=1)[S:3][C:2]([F:6])([F:5])[F:1]

Komponenten

4

Edukt 3

HCID 6344DichloromethaneHCID 67900Methanesulfenyl chloride, trifluoro-HCID 27574091-Chloro-4-(isocyanomethyl)benzene

Produkt 1

HCID 18930385Trifluoromethyl 1-chloro-N-(p-chlorobenzyl)thioformimidateAusbeute 68 %

Versuchsvorschrift

Trifluoromethylsulfenyl chloride (4.0 g, 0.03 mol) is bubbled over 30 minutes into a solution of 4-chlorobenzylisonitrile (3.0 g, 0.02 mol) in methylene chloride, causing the formation of a white precipitate. The suspension is stirred for 16 hours at room temperature and filtered to remove solids. The white filter cake is washed with methylene chloride and solvent is removed under reduced pressure to obtain an amber oil. Bulb-to-bulb distillation of the oil (90°-100° C., 0.05 mmHg) gives the title product as a colorless oil (3.9 g, 68%).

Aufarbeitung

  1. filtrationfiltered
  2. customto remove solids
  3. washThe white filter cake is washed with methylene chloride and solvent
  4. customis removed under reduced pressure
  5. customto obtain an amber oil
  6. distillationBulb-to-bulb distillation of the oil (90°-100° C., 0.05 mmHg)

Quellen und Nachweise

ORD-Eintrag
ord-ad5fc0c2af754edcbfdc8a065345f3fb
Quelldatensatz
uspto-grants-1995_11
Patentnummer
US05468877

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