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Methanol → 1-(beta-Hydroxy-ethyl)-5-phenyl-7-chloro-1H-1,5-benzodiazepine-2,4-(3H,5H)-dione

HRID 1283338
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1283338
[C:1]1([N:7]2[C:13]3[CH:14]=[C:15]([Cl:18])[CH:16]=[CH:17][C:12]=3[NH:11][C:10](=[O:19])[CH2:9][C:8]2=[O:20])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO.[CH2:23]1[O:25][CH2:24]1.[OH-].C([N+](C)(C)C)C1C=CC=CC=1>O>[OH:25][CH2:24][CH2:23][N:11]1[C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=2[N:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[C:8](=[O:20])[CH2:9][C:10]1=[O:19]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 887MethanolHCID 6354Ethylene OxideHCID 66854Benzyltrimethylammonium hydroxideHCID 89657Desmethylclobazam

Produkt 1

HCID 215171751-(beta-Hydroxy-ethyl)-5-phenyl-7-chloro-1H-1,5-benzodiazepine-2,4-(3H,5H)-dione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962
Water
Lösungsmittel

Versuchsvorschrift

A mixture consisting of 28.6 gm (0.1 mol) of 5-phenyl-7-chloro-1H-1,5-benzodiazepine-2,4-(3H,5H)-dione, 500 ml of methanol, 25 ml of water, 10-15 ml of ethyleneoxide and 1 ml of Triton B (methanolic 35% solution of benzyl trimethylammonium hydroxide) was stirred at room temperature for about eight hours. Thereafter, the clear solution formed thereby was evaporated, the residue was taken up in methylene chloride, and the resulting solution was extracted with water, dried and evaporated. The residue was recrystallized from ethanol, yielding 25.6 gm (78% of theory) of the colorless crystalline compound of the formula ##SPC6##

Aufarbeitung

  1. customThereafter, the clear solution formed
  2. customthereby was evaporated
  3. extractionthe resulting solution was extracted with water
  4. customdried
  5. customevaporated
  6. customThe residue was recrystallized from ethanol
  7. customyielding 25.6 gm (78% of theory) of the colorless crystalline compound of the formula

Quellen und Nachweise

ORD-Eintrag
ord-52a45b361d134fbdbe957583f0861db4
Quelldatensatz
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
USRE028935

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