Water → 2,4,5-Trifluoro-6-n-butylthioisophthalonitrile

HRID 65459

Reaktionsgleichung

Reaktionsgleichung von HRID 65459
F[C:2]1[C:7]([C:8]#[N:9])=[C:6]([F:10])[C:5]([C:11]#[N:12])=[C:4]([F:13])[C:3]=1[F:14].[F-].[K+].[CH2:17]([SH:21])[CH2:18][CH2:19][CH3:20].O>C(#N)C>[F:10][C:6]1[C:5]([C:11]#[N:12])=[C:4]([F:13])[C:3]([F:14])=[C:2]([S:21][CH2:17][CH2:18][CH2:19][CH3:20])[C:7]=1[C:8]#[N:9]

Komponenten

6

Edukt 4

HCID 962WaterHCID 8012ButanethiolHCID 522689Potassium FluorideHCID 608182Tetrafluoroisophthalonitrile

Produkt 1

HCID 137155572,4,5-Trifluoro-6-n-butylthioisophthalonitrileAusbeute 77 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A 2.0 g amount of tetrafluoroisophthalonitrile and 0.87 g of potassium fluoride were dissolved in 10 ml of acetonitrile. After cooling to a temperature of 0° C., 0.90 g (1.04 ml) of n-butylmercaptan was gradually dropwise added to the mixture and the resultant mixture was stirred at a temperature of 0° C. or less for 12 hours. After 50 ml of water was added to the reaction mixture, the reaction mixture was extracted with chloroform and the extract was then washed with a saturated aqueous sodium bicarbonate solution, followed by drying with anhydrous magnesium sulfate. After distilling off the chloroform, the resultant crude product was distilled in vacuo. Thus, 2.08 g (77% yield) of the desired compound No. 52 was obtained.

Aufarbeitung

  1. additionwas gradually dropwise added to the mixture
  2. extractionthe reaction mixture was extracted with chloroform
  3. washthe extract was then washed with a saturated aqueous sodium bicarbonate solution
  4. dry with materialby drying with anhydrous magnesium sulfate
  5. distillationAfter distilling off the chloroform
  6. distillationthe resultant crude product was distilled in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-e74146e7cdd844159bbd849f6eebbb86
Quelldatensatz
uspto-grants-1986_09
Patentnummer
US04614742

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