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

HRID 2050754Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2050754
[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-109ff9f5073a42a199913f5aa92a7e46
Quelldatensatz
uspto-grants-1991_05
Patentnummer
US05015260

Notizen zur Reaktion

Wird geladen…