Sodium Hydroxide → 2-(2-Amino-phenoxy)-ethanol

HRID 1954662Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1954662
[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N+:11]([O-])=O.Cl[Sn]Cl.[Sn].[OH-].[Na+]>Cl.O>[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH2:11]

Komponenten

7

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

8.9 g (48.59 mmol) 2-(2-hydroxyethoxy)nitrobenzene A2, 16.44 g (72.88 mmol) SnCl2. 2H2O and 17.3 g (145.77 mmol) tin were stirred in 30.84 ml aqueous HCl (30%) and 25 ml water at 90° C. for 8 hours. After cooling, the solution was treated with aqueous 5n sodium hydroxide solution and stirred for 3 hours at 90° C. The aqueous solution was subsequently decanted, wherein, upon cooling, the crude product crystallized out and was removed by suction. This crude product was then taken up in methanol, warmed and the suspension was filtered. The filtrate was then concentrated in vacuo. 6 g of light-brown crystals were obtained; yield 80%.

Aufarbeitung

  1. temperatureAfter cooling
  2. customThe aqueous solution was subsequently decanted
  3. temperaturewherein, upon cooling
  4. customthe crude product crystallized out
  5. customwas removed by suction
  6. temperaturewarmed
  7. filtrationthe suspension was filtered
  8. concentrationThe filtrate was then concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-a72711845d1344cf888d5e64c5a6d13f
Quelldatensatz
uspto-grants-2000_09
Patentnummer
US06124135

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