Water → 7-Chloro-3-[[(tert-butylamino)oxy]carbonyl]pyrazolo[3,4-c][1]benzazepine-4,10(1H,9H)-dione

HRID 1954736

Reaktionsgleichung

Reaktionsgleichung von HRID 1954736
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]2[C:6](=[O:18])[C:7]3[C:14]([C:15]([OH:17])=[O:16])=[N:13][NH:12][C:8]=3[C:9](=[O:11])[NH:10][C:4]=2[CH:3]=1.C(N1C=CN=C1)(N1C=CN=C1)=O.Cl.[C:34]([NH:38]O)([CH3:37])([CH3:36])[CH3:35].O>CN(C)C=O>[Cl:1][C:2]1[CH:20]=[CH:19][C:5]2[C:6](=[O:18])[C:7]3[C:14]([C:15]([O:17][NH:38][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:16])=[N:13][NH:12][C:8]=3[C:9](=[O:11])[NH:10][C:4]=2[CH:3]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 682631,1'-CarbonyldiimidazoleHCID 2777896N-tert-butylhydroxylamine hydrochlorideHCID 178524941HCID 178524941, Verbindung2×

Produkt 1

HCID 1784499477-Chloro-3-[[(tert-butylamino)oxy]carbonyl]pyrazolo[3,4-c][1]benzazepine-4,10(1H,9H)-dioneAusbeute 61 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 7-chloro-3-(carboxy)pyrazolo[3,4-cl[1]-benzazepine-4,10(1H,9H)-dione (400 mg, 1.37 mmol) (compound of Example 9) and 1,1'-carbonyldiimidazole (334 mg, 2.06 mmol) in N,N-dimethylformamide (16 mL) was stirred for 1 hour. In one portion, N-tert-butylhydroxylamine hydrochloride (516 mg, 4.11 mmol) was added and the solution was stirred for 17 hours at room temperature. To the resulting solution was added water (20 mL). The insoluble material was filtered and washed with hot methanol (3×20 mL) to give the title compound (300 mg, 61% yield, m.p. 258° C.).

Aufarbeitung

  1. filtrationThe insoluble material was filtered
  2. washwashed with hot methanol (3×20 mL)

Quellen und Nachweise

ORD-Eintrag
ord-32c1229165db43d5bc5029c091e8139d
Quelldatensatz
uspto-grants-2000_09
Patentnummer
US06124281

Verknüpfte Notizen

Wird geladen…