Hydroxyamine hydrochloride → 5-p-Methoxybenzyloxy-1-hydroxy-2-hydroxymethyl-4-pyridone

HRID 1086179Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1086179
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([CH2:7][O:8][C:9]2[C:10](=[O:17])[CH:11]=[C:12]([CH2:15][OH:16])O[CH:14]=2)=[CH:5][CH:4]=1.Cl.[NH2:21][OH:22]>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([CH2:7][O:8][C:9]2[C:10](=[O:17])[CH:11]=[C:12]([CH2:15][OH:16])[N:21]([OH:22])[CH:14]=2)=[CH:5][CH:4]=1

Komponenten

4

Edukt 2

HCID 443297Hydroxyamine hydrochlorideHCID 104916984H-Pyran-4-one, 2-(hydroxymethyl)-5-[(4-methoxyphenyl)methoxy]-

Produkt 1

HCID 107076455-p-Methoxybenzyloxy-1-hydroxy-2-hydroxymethyl-4-pyridone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

39.3 g of 5-p-methoxybenzyloxy-2-hydroxymethyl-4-pyrone is dissolved in 600 ml of pyridine, then 52.2 g of hydroxylamine hydrochloride is added thereto, and reacted at 70°-75° C. for 2.5 hours. After the reaction, the reaction mixture is concentrated to about 100 ml and, after adding 100 ml of water thereto, added to a mixed solution of 75 ml of hydrochloric acid and 225 ml of water with ice cooling. The pH is adjusted to 2-2.5, and stirring is conducted at the same temperature for 30 minutes. The formed crystals are filtered off, washed with water and then dried to obtain 16.6 f of the title compound.

Aufarbeitung

  1. customreacted at 70°-75° C. for 2.5 hours
  2. customAfter the reaction
  3. concentrationthe reaction mixture is concentrated to about 100 ml
  4. additionafter adding 100 ml of water
  5. additionadded to a mixed solution of 75 ml of hydrochloric acid and 225 ml of water with ice cooling
  6. filtrationThe formed crystals are filtered off
  7. washwashed with water
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f5208b1528f84175a7e947960fac2e2b
Quelldatensatz
uspto-grants-1991_07
Patentnummer
US05028601

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