Isopropanol → Medazepam

HRID 262945

Reaktionsgleichung

Reaktionsgleichung von HRID 262945
[CH3:1][CH2:2][N:3]([CH3:19])[C:4]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:5]=1[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=O.C1N2CN3CN(C2)C[N:21]1C3.[Br-].[NH4+].C(O)(C)C>O>[Cl:18][C:15]1[CH:16]=[CH:17][C:4]2[N:3]([CH3:19])[CH2:2][CH2:1][N:21]=[C:6]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[C:5]=2[CH:14]=1

Komponenten

6

Edukt 4

HCID 3776IsopropanolHCID 4101HexamethylenetetramineHCID 25514Ammonium BromideHCID 571010882-(2-Ethyl-methylamino)-5-chlorobenzophenone

Produkt 1

HCID 4041Medazepam

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Reflux 0.005 moles of 2-(2-ethyl-methylamino)-5-chlorobenzophenone, 0.020 moles of hexamethylenetetramine and 0.020 moles of ammonium bromide together for 2 hours in 14 ml. of 85% (v/v) aqueous isopropyl alcohol. Pour the reaction mixture into water and extract the product with benzene. Wash the benzene solution with water, dry over anhydrous sodium sulfate, filter and evaporate to dryness. After recrystallization, 7-chloro-2,3-dihydro-1-methyl-5-phenyl-1H-1,4-benzodiazepine is obtained. The material gives a single spot by thin layer chromatography, and after drying under vacuum at 110° C., shows no depression on mixed melting point with an authentic sample.

Aufarbeitung

  1. extractionextract the product with benzene
  2. washWash the benzene solution with water
  3. dry with materialdry over anhydrous sodium sulfate
  4. filtrationfilter
  5. customevaporate to dryness
  6. customAfter recrystallization

Quellen und Nachweise

ORD-Eintrag
ord-5985d48a684e429081cc14650201402b
Quelldatensatz
uspto-grants-1979_05
Patentnummer
US04155904

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