Ceric ammonium nitrate → HCID 21919159, Verbindung

HRID 1245201Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1245201
C[O:2][C:3]1[C:4]([CH3:33])=[C:5]([C:24]([O:31]C)=[C:25]([O:29][CH3:30])[C:26]=1[O:27][CH3:28])[CH2:6][C:7]1[CH:8]=[CH:9][C:10]([C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=2)=[C:11]([CH:15]=1)[C:12]([OH:14])=[O:13].O=[N+]([O-])[O-].[O-][N+](=O)[O-].[O-][N+](=O)[O-].[O-][N+](=O)[O-].[O-][N+](=O)[O-].[O-][N+](=O)[O-].[Ce+4].[NH4+].[NH4+]>C(#N)C.O>[CH3:28][O:27][C:26]1[C:3](=[O:2])[C:4]([CH3:33])=[C:5]([CH2:6][C:7]2[CH:8]=[CH:9][C:10]([C:16]3[CH:17]=[CH:18][C:19]([O:22][CH3:23])=[CH:20][CH:21]=3)=[C:11]([CH:15]=2)[C:12]([OH:14])=[O:13])[C:24](=[O:31])[C:25]=1[O:29][CH3:30]

Komponenten

5

Edukt 2

HCID 180504Ceric ammonium nitrateHCID 121472845-(3,4,5,6-Tetramethoxy-2-methylbenzyl)-2-(4-methoxyphenyl)benzoic acid

Produkt 1

HCID 21919159HCID 21919159, VerbindungAusbeute 63 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

5-(3,4,5,6-Tetramethoxy-2-methylbenzyl)-2-(4-methoxy-phenyl)benzoic acid (440 mg, 0.9734 mmol) was dissolved in a mixed solvent of acetonitrile (30 ml) and water (10 ml), then CAN (1.10 g, 2.0072 mmol) was added thereto at room temperature and the mixture was stirred for 3 hour. The reaction solution was poured into water and extracted with ether. The extract was washed with water and dried and the solvent was evaporated therefrom. The residue was purified by silica gel column chromatography (5% methanol-methylene chloride) to give the title compound (259 mg, 0.6137 mmol, 63%).

Aufarbeitung

  1. extractionextracted with ether
  2. washThe extract was washed with water
  3. customdried
  4. customthe solvent was evaporated
  5. customThe residue was purified by silica gel column chromatography (5% methanol-methylene chloride)

Quellen und Nachweise

ORD-Eintrag
ord-582bf45822c44a6ea99578ed50cfd7d4
Quelldatensatz
uspto-grants-2006_10
Patentnummer
US07122543B2

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