Hydrogen Bromide → 2,3-dihydro-4-fluoro-2-(4-pyridinylamino)-1H-isoindol-5-ol hydrobromide

HRID 612479

Reaktionsgleichung

Reaktionsgleichung von HRID 612479
[F:1][C:2]1[C:10]([O:11]C)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH2:4][N:5]([NH:13][C:14]1[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=1)[CH2:6]2.[BrH:20]>O>[BrH:20].[F:1][C:2]1[C:10]([OH:11])=[CH:9][CH:8]=[C:7]2[C:3]=1[CH2:4][N:5]([NH:13][C:14]1[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=1)[CH2:6]2

Komponenten

4

Edukt 2

HCID 260Hydrogen BromideHCID 195951342,3-Dihydro-4-fluoro-5-methoxy-N-(4-pyridinyl)-1H-isoindol-2-amine

Produkt 1

HCID 195952012,3-dihydro-4-fluoro-2-(4-pyridinylamino)-1H-isoindol-5-ol hydrobromideAusbeute 69 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 2,3-dihydro-4-fluoro-5-methoxy-N-(4-pyridinyl)-1H-isoindol-2-amine (3.25 g) in 48% hydrobromic acid (25 ml) was stirred, under reflux, for 5 hrs. The reaction mixture was diluted with water and stirred at ambient temperature overnight. The mixture was cooled to approximately 10° C. and filtered. The filter cake was washed with cold water and dried under vacuum at 80° C. to give 2.8 g (69%) of product. Recrystallization from water gave the analytical sample, mp. >250° C., dried at 80° C. under vacuum.

Aufarbeitung

  1. temperatureunder reflux, for 5 hrs
  2. temperatureThe mixture was cooled to approximately 10° C.
  3. filtrationfiltered
  4. washThe filter cake was washed with cold water
  5. customdried under vacuum at 80° C.

Quellen und Nachweise

ORD-Eintrag
ord-0400c73362384427be9c7378d34ea783
Quelldatensatz
uspto-grants-1999_12
Patentnummer
US06004977

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