Hydrochloric Acid → 3-Chloro-6-iodopyrazine-2-carbonitrile

HRID 1487357Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1487357
[ClH:1].N[C:3]1[C:4]([C:10]#[N:11])=[N:5][C:6]([I:9])=[CH:7][N:8]=1.N([O-])=O.[Na+]>O>[Cl:1][C:3]1[C:4]([C:10]#[N:11])=[N:5][C:6]([I:9])=[CH:7][N:8]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 23668193Sodium Nitrite2×HCID 866805543-Amino-6-iodopyrazine-2-carbonitrile

Produkt 1

HCID 866805553-Chloro-6-iodopyrazine-2-carbonitrileAusbeute 44 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
-50 °C

Versuchsvorschrift

64.3 ml of hydrochloric acid is added at −5° C. to 7.7 g (31.3 mmol) of 3-amino-6-iodopyrazine-2-carbonitrile. At this temperature, a sodium nitrite solution (4.32 g, 62.6 mmol) dissolved in 9 ml of water is added to the reaction mixture and is stirred for 4 hours at −50° C. and then at room temperature overnight. Another equivalent of sodium nitrite is added to the reaction mixture and the precipitate formed is filtered, rinsed with water and dried at 50° C. to yield 3.65 g (44%) of 3-chloro-6-iodopyrazine-2-carbonitrile in the form of a beige solid.

Aufarbeitung

  1. additionis added to the reaction mixture
  2. customat room temperature
  3. customovernight
  4. customthe precipitate formed
  5. filtrationis filtered
  6. washrinsed with water
  7. customdried at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-f93cbc89c4664bffb5fa957a5b8f1248
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09428510B2

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