Dimethylformamide → 5-[4-(2-Propyl-3-chloro-4-acetylphenoxy)butyl]-tetrazole

HRID 34972

Reaktionsgleichung

Reaktionsgleichung von HRID 34972
[CH2:1]([C:4]1[C:15]([Cl:16])=[C:14]([C:17](=[O:19])[CH3:18])[CH:13]=[CH:12][C:5]=1[O:6][CH2:7][CH2:8][CH2:9][C:10]#N)[CH2:2][CH3:3].[N-:20]=[N+:21]=[N-:22].[CH3:23][N:24](C)C(=[NH2+])N(C)C.CN(C)C=O.C(OCC)(=O)C>O>[CH2:1]([C:4]1[C:15]([Cl:16])=[C:14]([C:17](=[O:19])[CH3:18])[CH:13]=[CH:12][C:5]=1[O:6][CH2:7][CH2:8][CH2:9][CH2:10][C:23]1[NH:24][N:22]=[N:21][N:20]=1)[CH2:2][CH3:3]

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 8857Ethyl AcetateHCID 212972634-(2-Propyl-3-chloro-4-acetylphenoxy)butane nitrileHCID 178484365HCID 178484365, Verbindung

Produkt 1

HCID 1784396765-[4-(2-Propyl-3-chloro-4-acetylphenoxy)butyl]-tetrazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 0.5 g. of 4-(2-propyl-3- chloro-4-acetylphenoxy)butane nitrile and 1.3 g. of tetramethylguanidinium azide in 3 ml. of dimethylformamide was heated overnight at 125° C. The reaction was cooled, ethyl acetate and water were added, and the layers were separated. Water was added to the ethyl acetate layer, the water layer was acidified, and the layers were separated. The ethyl acetate was dried and evaporated to dryness. The residue was purified by chromatography to give the desired title product. NMR.

Aufarbeitung

  1. temperatureThe reaction was cooled
  2. customthe layers were separated
  3. additionWater was added to the ethyl acetate layer
  4. customthe layers were separated
  5. dry with materialThe ethyl acetate was dried
  6. customevaporated to dryness
  7. customThe residue was purified by chromatography

Quellen und Nachweise

ORD-Eintrag
ord-7298b72149514b3780afca07e5e83947
Quelldatensatz
uspto-grants-1988_08
Patentnummer
US04764521

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