Sulfuric acid magnesium salt (1:1) → HCID 178519077, Verbindung

HRID 907842Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 907842
[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]2[C:3]=1[CH2:4][O:5][C:6]2=[O:12].[F:13][C:14]1[CH:21]=[CH:20][C:17]([CH:18]=O)=[CH:16][CH:15]=1.[O-]S([O-])(=O)=O.[Mg+2]>C(Cl)Cl>[F:11][C:9]1[CH:8]=[C:7]2[C:3]([CH2:4][O:5][C:6]2=[O:12])=[C:2](/[N:1]=[CH:18]/[C:17]2[CH:20]=[CH:21][C:14]([F:13])=[CH:15][CH:16]=2)[CH:10]=1

Komponenten

5

Edukt 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 680234-FluorobenzaldehydeHCID 672589744-Amino-6-fluoroisobenzofuran-1(3H)-one

Produkt 1

HCID 178519077HCID 178519077, VerbindungAusbeute 34,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

4-amino-6-fluoroisobenzofuran-1(3H)-one (1.5 g, 8.98 mmol), 4-fluorobenzaldehyde (1.67 g, 13.47 mmol) and 12.75 g of MgSO4 were added into 40 ml of DCM and stirred under reflux overnight, then the mixture was evaporated under reduced pressure and the residues was dried in vacuum. 850 mg of (E)-6-fluoro-4-(4-fluorobenzylideneamino)isobenzofuran-1(3H)-one was obtained. 1H-NMR (400 MHz, CDCl3) δ (ppm): 5.37 (s, 2); 7.09-7.12 (dd, 1H), 7.19-7.23 (t, 2H), 7.43-7.45 (dd, 1H), 7.92-7.95 (m, 2H), 8.49 (s, 1H); LC-MS (ESI) m/z: 274 (M+1)+.

Aufarbeitung

  1. temperatureunder reflux overnight
  2. customthe mixture was evaporated under reduced pressure
  3. customthe residues was dried in vacuum

Quellen und Nachweise

ORD-Eintrag
ord-d513d0e3ecfe43c4b4c47c72747ae0dc
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08012976B2

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