Hydrochloric Acid → HCID 178419015, Verbindung

HRID 356797

Reaktionsgleichung

Reaktionsgleichung von HRID 356797
[C:1]([C:5]1[CH:12]=[CH:11][C:8]([C:9]#[N:10])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[Cl-].[Li+].[N-:15]=[N+:16]=[N-:17].[Na+].[Br-].C([NH+](CC)CC)C.Cl>CN(C=O)C.O>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([C:9]2[NH:17][N:16]=[N:15][N:10]=2)=[CH:11][CH:12]=1)([CH3:4])([CH3:2])[CH3:3]

Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 12493Triethylamine hydrobromideHCID 33557Sodium AzideHCID 778834-tert-ButylbenzonitrileHCID 433294Lithium Chloride

Produkt 1

HCID 178419015HCID 178419015, VerbindungAusbeute 70,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

In a 250 ml round-bottomed flask fitted with reflux condenser, 4.9 g of p-t-butylbenzonitrile, 3.82 g of lithium chloride and 5.85 g of sodium azide and 8.2 g of triethylammonium bromide in 100 ml of DMF are heated at 120° C. for 8 hours. After cooling to room temperature, 100 ml of water are added and the mixture is admixed in an ice bath with dilute hydrochloric acid until no further solid precipitates. The precipitate is filtered off with suction, washed with water and dried. Recrystallization from ethanol/water gives 4.4 g of colorless crystals.

Aufarbeitung

  1. customIn a 250 ml round-bottomed flask fitted
  2. temperaturewith reflux condenser
  3. customprecipitates
  4. filtrationThe precipitate is filtered off with suction
  5. washwashed with water
  6. customdried
  7. customRecrystallization from ethanol/water

Quellen und Nachweise

ORD-Eintrag
ord-31833a1e0ad14612875a81cff3bd5702
Quelldatensatz
uspto-grants-1998_11
Patentnummer
US05840217

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