Hydrochloric Acid → HCID 178419015, Verbindung

HRID 635127

Reaktionsgleichung

Reaktionsgleichung von HRID 635127
[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, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

4.99 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 were heated at 120° C. for 8 h in a 250 ml round-bottom flask fitted with a reflux condenser. After cooling to room temperature, 100 ml of water were added, and, in an ice bath, dilute hydrochloric acid was added until no more precipitate formed. The mixture was filtered with suction, and the precipitate was washed with water and dried. Recrystallization from ethanol/water produced 4.4 g of colorless crystals.

Aufarbeitung

  1. customfitted with a reflux condenser
  2. customformed
  3. filtrationThe mixture was filtered with suction
  4. washthe precipitate was washed with water
  5. customdried
  6. customRecrystallization from ethanol/water

Quellen und Nachweise

ORD-Eintrag
ord-0561e6e8c8e64a3dac1e01782ec069c9
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06187224B1

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