Hydrochloric Acid → HCID 178458271, Verbindung

HRID 1863134Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1863134
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([O:19][CH2:20][CH2:21][CH3:22])=[C:7]([C:9]2[N:17]=[C:16]3[C:12](=[N:13][N:14]=[N:15]3)[C:11](=[O:18])[N:10]=2)[CH:8]=1)#[N:2].[N-:23]=[N+:24]=[N-:25].[Na+].[Cl-].[NH4+].Cl>O.CN1CCCC1=O>[CH2:20]([O:19][C:6]1[CH:5]=[CH:4][C:3]([C:1]2[NH:25][N:24]=[N:23][N:2]=2)=[CH:8][C:7]=1[C:9]1[N:17]=[C:16]2[C:12](=[N:13][N:14]=[N:15]2)[C:11](=[O:18])[N:10]=1)[CH2:21][CH3:22]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 20392959HCID 20392959, Verbindung

Produkt 1

HCID 178458271HCID 178458271, VerbindungAusbeute 28,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Versuchsvorschrift

A mixture of 2-(5-cyano-2-propoxyphenyl)-8-azapurin-6-one (2.0 g), sodium azide (1.05 g), ammonium chloride (0.9 g) and N-methylpyrrolid-2-one (16 ml) was cautiously heated, with stirring, in a sealed flask for 7 hours at 100°-110° C. The mixture was then cooled and added to water (80 ml) and the mixture was acidified by treatment with concentrated hydrochloric acid. The solid which separated was filtered off and recrystallised from acetic acid to give 2-[2-propoxy-5-(tetrazol-5-yl)phenyl]-8-azapurin-6-one (0.65 g), m.p. 253°-259° C. (with decomposition).

Aufarbeitung

  1. temperaturewas cautiously heated
  2. temperatureThe mixture was then cooled
  3. customThe solid which separated
  4. filtrationwas filtered off
  5. customrecrystallised from acetic acid

Quellen und Nachweise

ORD-Eintrag
ord-11347122a2064313a7993610cc1356b9
Quelldatensatz
uspto-grants-1979_09
Patentnummer
US04167568

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