Water → Phenol, 5-[(2-hydroxyethyl)amino]-4-methoxy-2-methyl-

HRID 1029997Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1029997
[OH-].[Na+].[CH3:3][O:4][C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([OH:12])=[CH:7][C:6]=1[N:13]1[CH2:17][CH2:16][O:15]C1=O.O>C(O)(=O)C>[CH3:11][C:9]1[CH:10]=[C:5]([O:4][CH3:3])[C:6]([NH:13][CH2:17][CH2:16][OH:15])=[CH:7][C:8]=1[OH:12]

Komponenten

5

Edukt 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 19821132HCID 19821132, Verbindung

Produkt 1

HCID 9794190Phenol, 5-[(2-hydroxyethyl)amino]-4-methoxy-2-methyl-Ausbeute 45,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

10 ml of 5N sodium hydroxide was heated to 70° C., and 2.76 g (12.4 mmol) of N-(2-methoxy-4-methyl-5-hydroxyphenyl)-1,3-oxazolidin-2-one was added thereto, and then the resulting mixture was stirred at 70° C. for 1 hour. After allowing to cool, 40 ml of water was poured into the reaction mixture, and acetic acid was added thereto until no further crystals were precipitated. The crystals were filtered, washed with water and recrystallized from the solvent mixture of water/ethanol (4:1, by volume). Thus, 1.10 g (5.6 mmol) of 2-methyl-4-methoxy-5-(β-hydroxyethylamino)phenol was obtained. The yield was 45%.

Aufarbeitung

  1. temperatureto cool
  2. additionwas added
  3. customuntil no further crystals were precipitated
  4. filtrationThe crystals were filtered
  5. washwashed with water
  6. customrecrystallized from the solvent mixture of water/ethanol (4:1, by volume)

Quellen und Nachweise

ORD-Eintrag
ord-a04b393520c14199922277890d2a3cfc
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05104414

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