Potassium Hydroxide → HCID 20394577, Verbindung

HRID 261699Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 261699
[OH-].[K+].C([O-])C.C[O:7][C:8]([C:10]1[N:11]([CH3:33])[C:12](=[O:32])[N:13]2[C:19]3[CH:20]=[CH:21][C:22]([Cl:24])=[CH:23][C:18]=3[C:17]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=3[Cl:31])=[N:16][CH2:15][C:14]=12)=[O:9]>O.CO>[Cl:24][C:22]1[CH:21]=[CH:20][C:19]2[N:13]3[C:12](=[O:32])[N:11]([CH3:33])[C:10]([C:8]([OH:9])=[O:7])=[C:14]3[CH2:15][N:16]=[C:17]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=3[Cl:31])[C:18]=2[CH:23]=1

Komponenten

5

Edukt 2

HCID 14797Potassium HydroxideHCID 867361548-chloro-6-(2-chlorophenyl)-1,2-dihydro-2-methyl-1-oxo-4H-imidazo[1,5-a][1,4]benzodiazepin-3-carboxylic acid methyl ester ethanolate

Produkt 1

HCID 20394577HCID 20394577, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

Potassium hydroxide, 1.3 g (0.02 mole), was dissolved in 1 ml of water and added to a suspension of 4 g (0.0097 mole) of 8-chloro-6-(2-chlorophenyl)-1,2-dihydro-2-methyl-1-oxo-4H-imidazo[1,5-a][1,4]benzodiazepin-3-carboxylic acid methyl ester ethanolate in 200 ml of methanol. The solution was refluxed under argon for 3 hrs, concentrated at reduced pressure, diluted with cold water and acidified with acetic acid to give an off-white solid. The solid was washed with water and air dried on the funnel overnight to give crude end product. Recrystallization from ethanol/methylene chloride gave white crystals with mp 265°-267° (dec).

Aufarbeitung

  1. temperatureThe solution was refluxed under argon for 3 hrs
  2. concentrationconcentrated at reduced pressure
  3. additiondiluted with cold water
  4. customto give an off-white solid
  5. washThe solid was washed with water and air
  6. customdried on the funnel overnight
  7. customto give crude end product
  8. customRecrystallization from ethanol/methylene chloride
  9. customgave white crystals with mp 265°-267° (dec)

Quellen und Nachweise

ORD-Eintrag
ord-723cd01a0c694694aee3c6ac9f8a19e5
Quelldatensatz
uspto-grants-1979_08
Patentnummer
US04166185

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