Triethylamine hydrochloride → HCID 178506136, Verbindung

HRID 1924428Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1924428
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[C:5]#[N:6].[N-:13]=[N+:14]=[N-:15].[Na+].Cl.C(N(CC)CC)C>C1(C)C=CC=CC=1>[F:1][C:2]([F:11])([F:12])[C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[C:5]1[NH:15][N:14]=[N:13][N:6]=1

Komponenten

5

Edukt 3

HCID 11130Triethylamine hydrochlorideHCID 33557Sodium AzideHCID 679722-(Trifluoromethyl)benzonitrile

Produkt 1

HCID 178506136HCID 178506136, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

A vigorously stirred suspension of 2-(trifluoromethyl)benzonitrile (2-A) (6.34 g, 37 mmol), sodium azide (4.81 g, 74 mmol) and triethylamine hydrochloride (10.19 g, 74 mmol) in toluene (70 mL) was heated at 110° C. for 48 h. The mixture was cooled and extracted twice with water. The combined extracts were washed with hexane and brought to pH about 1 with concentrated HCl. The precipitate which formed was filtered, washed with water and dried to give 5-[2-(trifluoromethyl)phenyl]-1H-tetrazole (2-B).

Aufarbeitung

  1. temperatureThe mixture was cooled
  2. extractionextracted twice with water
  3. washThe combined extracts were washed with hexane
  4. customThe precipitate which formed
  5. filtrationwas filtered
  6. washwashed with water
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-d4a4c10ce4dc490b844a1ab037243215
Quelldatensatz
uspto-grants-2012_05
Patentnummer
US08178546B2

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