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Ethanol → (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylic acid

HRID 223338
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 223338
[Cl:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]3[CH2:23][CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:18]CC)=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].C(O)C>O>[Cl:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]3[CH2:23][CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([OH:18])=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1
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Komponenten

5

Edukt 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 53890667ethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]-benzodiazepine-1-carboxylate

Produkt 1

HCID 22828765(S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962
Water
Lösungsmittel

Versuchsvorschrift

15 g (43.4 mmol) of ethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate and 1.85 g (46.3 mmol) of sodium hydroxide are treated with 60 ml of ethanol and 10 ml of water, then heated to boiling under reflux for 45 minutes, the ethanol is subsequently distilled off in vacuo, the residue is treated with 46.5 ml of 1 N hydrochloric acid and left to stand in an ice-bath for 2 hours. The precipitated material is filtered off under suction, washed with water and dried to constant weight. There is obtained (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylic acid which has a decomposition point of 265°.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 45 minutes
  3. distillationthe ethanol is subsequently distilled off in vacuo
  4. additionthe residue is treated with 46.5 ml of 1 N hydrochloric acid
  5. waitleft
  6. filtrationThe precipitated material is filtered off under suction
  7. washwashed with water
  8. customdried to constant weight

Quellen und Nachweise

ORD-Eintrag
ord-5e7b6bb01037448aae908d1a673e76e6
Quelldatensatz
uspto-grants-1982_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04353827

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