2-Methylimidazole → Estazolam

HRID 1764513

Reaktionsgleichung

Reaktionsgleichung von HRID 1764513
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([NH:12][NH2:13])[CH2:9][N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1.Cl.[CH:22](N)=N.CC1NC=CN=1>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:22]=[N:13][N:12]=[C:10]3[CH2:9][N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1

Komponenten

5

Edukt 3

HCID 127492-MethylimidazoleHCID 10313058Methanimidamide, hydrochloride (1:1)HCID 123908747-Chloro-2-hydrazinyl-5-phenyl-3H-1,4-benzodiazepine

Produkt 1

HCID 3261Estazolam

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 2.8 parts of 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine, 2.4 parts of formamidine hydrochloride and 2.5 parts of 2-methylimidazole is fused at 160° C for 10 minutes. Water is added to the mixture, followed by extraction with methylene chloride. The methylene chloride layer is washed with water, dried over sodium sulfate and the solvent is evaporated, whereby 8-chloro-6-phenyl-4H-s-triazolo [4,3-a][1,4] benzodiazepine is yielded. Recrystallization from ethyl acetate yields colorless flakes melting at 226° C to 227° C.

Aufarbeitung

  1. extractionfollowed by extraction with methylene chloride
  2. washThe methylene chloride layer is washed with water
  3. dry with materialdried over sodium sulfate
  4. customthe solvent is evaporated

Quellen und Nachweise

ORD-Eintrag
ord-2f9d688256f6492a8e3493b7ddfa1c2a
Quelldatensatz
uspto-grants-1978_09
Patentnummer
US04116956

Verknüpfte Notizen

Wird geladen…