Ammonium Chloride → HCID 15341803, Verbindung

HRID 1033631Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1033631
[OH:1][C:2]1[C:11]([CH2:12][CH:13]=[CH2:14])=[C:10]([OH:15])[CH:9]=[CH:8][C:3]=1[C:4](OC)=[O:5].[Cl-].[NH4+:17]>C(O)C>[OH:1][C:2]1[C:11]([CH2:12][CH:13]=[CH2:14])=[C:10]([OH:15])[CH:9]=[CH:8][C:3]=1[C:4]([NH2:17])=[O:5]

Komponenten

4

Edukt 2

HCID 25517Ammonium ChlorideHCID 13019279Methyl 2,4-dihydroxy-3-(prop-2-en-1-yl)benzoate

Produkt 1

HCID 15341803HCID 15341803, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

Methyl 2,4-dihydroxy-3-(2-propenyl)benzoate (4.4 g) was added to a mixture of about 10 to 15 ml of saturated ammonium chloride solution and 2 to 3 ml of ethanol. The reaction mixture was stirred overnight at 50° C. The reaction mixture was extracted five times with ethyl acetate, and the organic layer was concentrated under vacuum. The product was crystallized and recrystallized from chloroform. Subsequent chromatography of the precipitated product on a 25 g silica gel column with 40% ethyl acetate/hexane as eluant gave the pure product.

Aufarbeitung

  1. extractionThe reaction mixture was extracted five times with ethyl acetate
  2. concentrationthe organic layer was concentrated under vacuum
  3. customThe product was crystallized
  4. customrecrystallized from chloroform
  5. customSubsequent chromatography of the precipitated product on a 25 g silica gel column with 40% ethyl acetate/hexane as eluant gave the pure product

Quellen und Nachweise

ORD-Eintrag
ord-474898591a7246b684160e620283ef73
Quelldatensatz
uspto-grants-1994_05
Patentnummer
US05310951

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