Hydrochloric Acid → 10-(5-aminomethyl-2-isoindolinyl)-9-fluoro-2,3-dihydro-3-methyl-7-oxo-7H-pyrido [1,2,3-de][1,4]-benzoxazine-6-carboxylic acid

HRID 1494813Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1494813
C([NH:4][CH2:5][C:6]1[CH:7]=[C:8]2[C:12](=[CH:13][CH:14]=1)[CH2:11][N:10]([C:15]1[C:16]([F:33])=[CH:17][C:18]3[C:28](=[O:29])[C:27]([C:30]([OH:32])=[O:31])=[CH:26][N:20]4[CH:21]([CH3:25])[CH2:22][O:23][C:24]=1[C:19]=34)[CH2:9]2)(=O)C.Cl.O.O1C2C=CC(C(O)=O)=CC=2C=CN1>C(O)C>[NH2:4][CH2:5][C:6]1[CH:7]=[C:8]2[C:12](=[CH:13][CH:14]=1)[CH2:11][N:10]([C:15]1[C:16]([F:33])=[CH:17][C:18]3[C:28](=[O:29])[C:27]([C:30]([OH:32])=[O:31])=[CH:26][N:20]4[CH:21]([CH3:25])[CH2:22][O:23][C:24]=1[C:19]=34)[CH2:9]2

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 21624997Benzoxazine-6-carboxylic acidHCID 6792243210-(5-acetamidomethyl-2-isoindolinyl)-9-fluoro-2,3-dihydro-3-methyl-7-oxo-7H-pyrido[1,2,3-de][1,4]-benzoxazine-6-carboxylic acid

Produkt 1

HCID 5424461510-(5-aminomethyl-2-isoindolinyl)-9-fluoro-2,3-dihydro-3-methyl-7-oxo-7H-pyrido [1,2,3-de][1,4]-benzoxazine-6-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

315 mg of 10-(5-acetamidomethyl-2-isoindolinyl)-9-fluoro-2,3-dihydro-3-methyl-7-oxo-7H-pyrido[1,2,3-de][1,4]-benzoxazine-6carboxylic acid was added to a mixed solution of 12 ml of concentrated HCl, 2.5 ml of water, and 5 ml of ethanol, and the mixture was heated under reflux for 15 hours. After the mixture was concentrated under reduced pressure, the residue was recrystallized from ethanol to obtain 170 mg of 10-(5-aminomethyl-2-isoindolinyl)-9-fluoro-2,3-dihydro-3-methyl-7-oxo-7H-pyrido[1,2,3-de]1,4]-benzoxazine-6-carboxylic acid.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 15 hours
  3. concentrationAfter the mixture was concentrated under reduced pressure
  4. customthe residue was recrystallized from ethanol
  5. customto obtain 170 mg of 10-(5-aminomethyl-2-isoindolinyl)-9-fluoro-2,3-dihydro-3-methyl-7-oxo-

Quellen und Nachweise

ORD-Eintrag
ord-cda002c69e774e60bcf6526a3b4298ac
Quelldatensatz
uspto-grants-1991_06
Patentnummer
US05026856

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