Hydrochloric Acid → HCID 10474189, Verbindung

HRID 1793823Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1793823
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([C:13]2[CH:18]=[C:17]([OH:19])[C:16]([O:20][CH3:21])=[CH:15][C:14]=2[CH:22]([CH2:26][CH3:27])[C:23](=O)[CH3:24])=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[NH2:28][NH2:29].Cl>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[C:13]3[CH:18]=[C:17]([OH:19])[C:16]([O:20][CH3:21])=[CH:15][C:14]=3[CH:22]([CH2:26][CH3:27])[C:23]([CH3:24])=[N:29][N:28]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 9321HydrazineHCID 222197323-[2-(3,4-Dimethoxybenzoyl)-4-hydroxy-5-methoxyphenyl]pentan-2-one

Produkt 1

HCID 10474189HCID 10474189, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 14 g of 3-{2-[(3,4-dimethoxyphenyl)carbonyl]-4-hydroxy-5-methoxyphenyl}pentan-2-one and 4.7 mL of hydrazine in 280 mL of ethanol was heated at reflux for 0.5 hr. After allowing the solution to cool to room temperature, it was saturated with HCl gas. The mixture was then concentrated to a volume of about 5 mL, basified with concentrated ammonium hydroxide, and extracted with methylene chloride. The combined methylene chloride extracts were dried and concentrated, and the residue recrystallized from ethyl acetate/hexane. Yield: 1.5 g

Aufarbeitung

  1. temperatureat reflux for 0.5 hr
  2. concentrationThe mixture was then concentrated to a volume of about 5 mL
  3. extractionextracted with methylene chloride
  4. dry with materialThe combined methylene chloride extracts were dried
  5. concentrationconcentrated
  6. customthe residue recrystallized from ethyl acetate/hexane

Quellen und Nachweise

ORD-Eintrag
ord-cf908bae29b7404681d8111d8162a2a9
Quelldatensatz
uspto-grants-2006_04
Patentnummer
US07022700B2

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