Water → HCID 12445399, Verbindung

HRID 1942155

Reaktionsgleichung

Reaktionsgleichung von HRID 1942155
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][C:11]1[CH:19]=[CH:18][C:14]2[O:15][CH2:16][O:17][C:13]=2[CH:12]=1)([O-])=O.C(OCC)(=O)C.O>[Fe].C(O)(=O)C>[O:15]1[C:14]2[CH:18]=[CH:19][C:11]([NH:10][C:5]3[C:4]([NH2:1])=[CH:9][CH:8]=[CH:7][CH:6]=3)=[CH:12][C:13]=2[O:17][CH2:16]1

Komponenten

6

Edukt 3

HCID 962WaterHCID 8857Ethyl AcetateHCID 7922985N-(2-nitrophenyl)benzo[d][1,3]dioxol-5-ylamine

Produkt 1

HCID 12445399HCID 12445399, VerbindungAusbeute 100,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

13.6 g (244 mmol) of iron powder and 10.5 g (40 mmol) of N-(2-nitrophenyl)benzo[d][1,3]dioxol-5-ylamine were added to a solvent mixture of ethyl acetate (130 ml), water (65 mL) and acetic acid (15 mL), and the mixture was stirred for 1 hour at 70° C. The reaction solution was cooled to room temperature, and the waste was separated by filtration using a filter aid. The organic layer of the filtrate was batched off, washed with water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 9.2 g (yield: 99%) of N-(benzo[d][1,3]dioxol-5-yl)benzene-1,2-diamine as white crystals.

Aufarbeitung

  1. temperatureThe reaction solution was cooled to room temperature
  2. customthe waste was separated by filtration
  3. washwashed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-99a30c1e35a34c6aa59cae89f80c859d
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08389523B2

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