Ammonium Chloride → 3-Methoxymethyloxy-1,2-benzenedimethanol

HRID 1064834

Reaktionsgleichung

Reaktionsgleichung von HRID 1064834
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][CH2:9][O:10][C:11]1[CH:21]=[CH:20][CH:19]=[C:13]2[C:14]([O:16][C:17](=O)[C:12]=12)=[O:15].[Cl-].[NH4+]>O1CCCC1.CCOCC>[CH3:7][O:8][CH2:9][O:10][C:11]1[CH:21]=[CH:20][CH:19]=[C:13]([CH2:14][OH:15])[C:12]=1[CH2:17][OH:16]

Komponenten

6

Edukt 3

HCID 25517Ammonium ChlorideHCID 21226445Aluminium lithium hydrideHCID 219367353-Methoxymethyloxyphthalic anhydride

Produkt 1

HCID 222728523-Methoxymethyloxy-1,2-benzenedimethanolAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

After that, lithium aluminum hydride (1.14 g, 30.0 mmol) was added little by little to a solution of 3-methoxymethyloxyphthalic anhydride (3.0 g, 14.4 mmol) in anhydrous tetrahydrofuran (100 ml) under cooling with ice water and the mixture was returned to room temperature followed by stirring for 12 hours. The reaction solution was diluted with ether (300 ml) and a saturated aqueous solution (3 ml) of ammonium chloride was added thereto followed by stirring for 1 hour. The reaction solution was dried over anhydrous magnesium sulfate, filtered off through celite and the filtrate was concentrated to provide 1.71 g (yield 60%) of 3-methoxymethyloxy-1,2-benzenedimethanol as colorless oil.

Aufarbeitung

  1. customwas returned to room temperature
  2. stirringby stirring for 1 hour
  3. dry with materialThe reaction solution was dried over anhydrous magnesium sulfate
  4. filtrationfiltered off through celite
  5. concentrationthe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-643fbb12b6c24edf9251de60c65dea63
Quelldatensatz
uspto-grants-2005_11
Patentnummer
US06969711B2

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