Sodium Hydroxide → 1,2,3,6-Tetrahydro-1-methyl-4-(2,4,6-trimethoxyphenyl)-3-pyridinol

HRID 2304805Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2304805
Br.Br[CH:3]1[C:8]([C:9]2[C:14]([O:15][CH3:16])=[CH:13][C:12]([O:17][CH3:18])=[CH:11][C:10]=2[O:19][CH3:20])=[CH:7][CH2:6][N:5]([CH3:21])[CH2:4]1.[OH-:22].[Na+]>O>[OH:22][CH:3]1[C:8]([C:9]2[C:14]([O:15][CH3:16])=[CH:13][C:12]([O:17][CH3:18])=[CH:11][C:10]=2[O:19][CH3:20])=[CH:7][CH2:6][N:5]([CH3:21])[CH2:4]1

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 9866952HCID 9866952, Verbindung

Produkt 1

HCID 99256571,2,3,6-Tetrahydro-1-methyl-4-(2,4,6-trimethoxyphenyl)-3-pyridinol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

50 g (0.118 mol of 3(R,S)-bromo-1-methyl-4-(2,4,6-trimethoxyphenyl)-1,2,3,6-tetrahydropyridine hydrobromide (VI) were heated under reflux for 2 h in 100 ml of water. The reaction mixture was then cooled to 20° C. and adjusted to pH 12.5 by dropwise addition of 30 ml of 30% strength sodium hydroxide solution. After a short time, a pale brown precipitate crystallized out. The mixture was stirred at 5-10° C. for a further 1 h, and the precipitated product was filtered off with suction and washed with 30 ml of water. The crude product was then stirred with 20 ml of acetone, filtered off with suction and dried in vacuo.

Aufarbeitung

  1. customAfter a short time, a pale brown precipitate crystallized out
  2. filtrationthe precipitated product was filtered off with suction
  3. washwashed with 30 ml of water
  4. stirringThe crude product was then stirred with 20 ml of acetone
  5. filtrationfiltered off with suction
  6. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-1a8b261ef9224735a513c0e567f765c9
Quelldatensatz
uspto-grants-2002_08
Patentnummer
US06437136B1

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