Ammonia → 2-Amino-3,6-difluorobenzonitrile

HRID 1418359Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1418359
F[C:2]1[C:9]([F:10])=[CH:8][CH:7]=[C:6]([F:11])[C:3]=1[C:4]#[N:5].O.[NH3:13]>C(#N)C>[NH2:13][C:2]1[C:9]([F:10])=[CH:8][CH:7]=[C:6]([F:11])[C:3]=1[C:4]#[N:5]

Komponenten

5

Edukt 3

HCID 222AmmoniaHCID 962WaterHCID 1456222,3,6-Trifluorobenzonitrile

Produkt 1

HCID 450905912-Amino-3,6-difluorobenzonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

2,3,6-Trifluorobenzonitrile (1.76 ml, 15.2 mmol) in aqueous ammonia (20 ml) and acetonitrile (10 ml) was stirred for 7 days. Water was added. The whole was extracted with ether, the ether was dried (sodium sulphate) and evaporated. Flash column chromatography on silica gel, eluting with dichloromethane, gave the product (1.2 g), MS (+EI) 154 (M+), 1H NMR (CDCl3) 7.07-7.16 (1H, m), 6.36-6.43 (1H, m), 4.62 (2H, s).

Aufarbeitung

  1. extractionThe whole was extracted with ether
  2. dry with materialthe ether was dried (sodium sulphate)
  3. customevaporated
  4. washFlash column chromatography on silica gel, eluting with dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-d58cefe9ca844147a6bbb301c478e1e4
Quelldatensatz
uspto-grants-1999_03
Patentnummer
US05883102

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