Nitrite → 3,4-Bistrifluoromethylbenzonitrile

HRID 1030088

Reaktionsgleichung

Reaktionsgleichung von HRID 1030088
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[C:5]([CH:7]=[CH:8][C:9]=1[C:10]([F:13])([F:12])[F:11])N.S(=O)(=O)(O)O.N([O-])=O.[Na+].N([O-])=O.[C-]#N.[Na+].[Cu][C:32]#[N:33].C(=O)([O-])O.[Na+]>O.S([O-])([O-])(=O)=O.[Ni+2]>[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[C:5]([CH:7]=[CH:8][C:9]=1[C:10]([F:13])([F:12])[F:11])[C:32]#[N:33]

Komponenten

10

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

229 g (1 mol) of 3,4-bistrifluoromethylaniline were diazotized in a solution of 350 g of concentrated sulphuric acid in 1.25 1 of water using 70 g of sodium nitrite in 140 ml of water. After the diazonium salt solution became nitrite-free, it was added dropwise to a solution warmed to 100° C. consisting of 550 ml of water, 210 g of sodium cyanide, 10 g of copper(I) cyanide, 500 g of sodium hydrogencarbonate and 9 g of nickel sulphate x 7 H2O. The product was isolated from the reaction mixture by steam distillation and subsequently distilled again. 152 g of product having a boiling point at 14 mbar of 85° C. and a melting point of 71° to 72° C. were obtained. This corresponds to a yield of 63% of theory.

Aufarbeitung

  1. additionwas added dropwise to a solution
  2. customThe product was isolated from the reaction mixture by steam distillation
  3. distillationsubsequently distilled again
  4. customat 14 mbar of 85° C.
  5. customa melting point of 71° to 72° C. were obtained

Quellen und Nachweise

ORD-Eintrag
ord-f1a102762c8d4bacaa5cfc848c290756
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05104879

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