Water → P-Anisidine

HRID 541167

Reaktionsgleichung

Reaktionsgleichung von HRID 541167
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-])=O)=[CH:5][CH:4]=1.O>C(OCC)(=O)C>[NH2:9][C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1

Komponenten

4

Versuchsvorschrift

76.6 mg (0.50 mmol) of 1-methoxy-4-nitrobenzene (10), 270 μL (15 mmol) of distilled water and stainless steel balls (50 pieces) were placed in the vessel of the planetary ball mill, which was then closed, and agitated by operating the planetary ball mill for 12 hours at 800 rpm (reversed every 30 minutes). After the lapse of 12 hours, 10 mL of ethyl acetate was added to the vessel of the ball mill to provide a solution containing the reaction mixture, which was then filtered with celite. The operation was repeated 5 times to provide a filtrate, which was then concentrated, thereby providing 48.2 mg (0.39 mmol) of 4-amino-1-methoxybenzene (11). The yield was 78%. The reaction is expressed by the following scheme.

Aufarbeitung

  1. customwas then closed
  2. customfor 12 hours
  3. customto provide a solution
  4. additioncontaining the reaction mixture, which
  5. filtrationwas then filtered with celite
  6. customto provide a filtrate, which
  7. concentrationwas then concentrated

Quellen und Nachweise

ORD-Eintrag
ord-86bfe732eb444b93b9770f5c5d788060
Quelldatensatz
uspto-grants-2014_10
Patentnummer
US08871980B2

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