Water → HCID 178420099, Verbindung

HRID 972550Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 972550
[C:1]1([C:7]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)([CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][CH:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:14][CH2:13]2)[C:8]#[N:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.[N-:31]=[N+:32]=[N-:33].[Na+]>CN(C)C=O.[Cl-].[NH4+].[Cl-].[Li+]>[C:1]1([C:7]([C:8]2[NH:33][N:32]=[N:31][N:9]=2)([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][CH:15]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH2:14][CH2:13]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Komponenten

7

Edukt 3

HCID 962WaterHCID 33557Sodium AzideHCID 214047972,2-Diphenyl-4-(4-phenylpiperidino)butyronitrile

Produkt 1

HCID 178420099HCID 178420099, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6228DimethylformamideLösungsmittelHCID 25517Ammonium ChlorideLösungsmittelHCID 433294Lithium ChlorideLösungsmittel

Versuchsvorschrift

11.0 Parts of 2,2-diphenyl-4-(4-phenylpiperidino)butyronitrile are dissolved in 55 parts by volume of dimethylformamide along with 2.82 parts of sodium azide, 2.32 parts of ammonium chloride and 0.04 parts of lithium chloride. This mixture is heated under a nitrogen atmosphere, in an oil bath which is kept at 125° C. The solution is cooled and poured into water which caused the formation of a gummy precipitate. The solvent phase is decanted from the gum. The gum is then crystallized from a mixture of methanol-ether and dried in vacuum to provide an off-white solid which is recrystallized from a mixture of methanol-ether and again dried in vacuum to provide 5-[1,1-diphenyl-3-(4-phenylpiperidino)propyl]-1H-tetrazole hemimethanolate, melting at 149° - 157° C. and having the following formula ##STR8##

Aufarbeitung

  1. temperatureThis mixture is heated under a nitrogen atmosphere, in an oil bath which
  2. customis kept at 125° C
  3. temperatureThe solution is cooled
  4. customThe solvent phase is decanted from the gum
  5. customThe gum is then crystallized from a mixture of methanol-ether
  6. customdried in vacuum
  7. customto provide an off-white solid which
  8. customis recrystallized from a mixture of methanol-ether
  9. customagain dried in vacuum

Quellen und Nachweise

ORD-Eintrag
ord-b5779c0e6f5340a0a8606def85790994
Quelldatensatz
uspto-grants-1977_10
Patentnummer
US04053477

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