Sodium Hydroxide → HCID 22247174, Verbindung

HRID 1815943Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1815943
[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([CH:22]=[O:23])=[C:13]([N:15]([CH2:18][CH:19]([OH:21])[CH3:20])C=O)[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>C1COCC1>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([CH:22]=[O:23])=[C:13]([NH:15][CH2:18][CH:19]([OH:21])[CH3:20])[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 22247178N-(5-Benzyloxy-2-formylphenyl)-N-(2-hydroxypropyl)-formamide

Produkt 1

HCID 22247174HCID 22247174, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

An ice-cooled solution of the product from Step B (298 g, 0.95 mol) in THF (3 L) was treated with 1 M aqueous sodium hydroxide (1.95 L, 1.9 mol) keeping the temperature below 8° C. After the starting material was consumed, the mixture was diluted with brine and extracted twice with ethyl ether. The organic solution was washed with water until neutral and then with brine, dried over sodium sulfate, treated with charcoal and passed through silica (1 kg) with ether and with 1:1 ethyl acetate-hexane to yield, after concentration in vacuo, a yellow solid (207 g, 76%).

Aufarbeitung

  1. customthe temperature below 8° C
  2. customAfter the starting material was consumed
  3. additionthe mixture was diluted with brine
  4. extractionextracted twice with ethyl ether
  5. washThe organic solution was washed with water until neutral and then with brine
  6. dry with materialdried over sodium sulfate
  7. additiontreated with charcoal
  8. customto yield
  9. concentrationafter concentration in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-1734a58b96084e46b7cdbcc4e74eae4d
Quelldatensatz
uspto-grants-2005_04
Patentnummer
US06881749B2

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