Dimethyl Sulfate → HCID 2825022, Verbindung

HRID 1073375Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1073375
[OH-].[Na+].S(OC)(O[CH3:7])(=O)=O.[OH:10][C:11]1[C:20]([CH3:21])=[C:19]2[C:14]([C:15](=[O:24])[CH2:16][C:17]([CH3:23])([CH3:22])[O:18]2)=[CH:13][CH:12]=1>O>[CH3:7][O:10][C:11]1[C:20]([CH3:21])=[C:19]2[C:14]([C:15](=[O:24])[CH2:16][C:17]([CH3:22])([CH3:23])[O:18]2)=[CH:13][CH:12]=1

Komponenten

5

Edukt 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 27279747-Hydroxy-2,2,8-trimethyl-2,3-dihydro-4H-1-benzopyran-4-one

Produkt 1

HCID 2825022HCID 2825022, VerbindungAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

The reaction is carried out under nitrogen. In 50 ml of a 10% sodium hydroxide solution 4.9 g (23.8 millimoles) of 7-hydroxy-2,2,8-trimethyl-4-chromanone are dissolved, 2.6 g (2 ml, 21 millimoles) of dimethyl sulfate are added and the reaction mixture is vigorously stirred for 2 hours. The reaction mixture is diluted with 100 ml of icecold water and extracted three times with 50 ml of carbon tetrachloride each. The organic phase is washed twice with 50 ml of water each, dried over sodium sulfate, the solvent is removed and the residue crystallized from 90% methanol. Thus 3.4 g of the desired compound are obtained, yield 78%. Mp.: 105°-107° C.

Aufarbeitung

  1. extractionextracted three times with 50 ml of carbon tetrachloride each
  2. washThe organic phase is washed twice with 50 ml of water each,
  3. dry with materialdried over sodium sulfate
  4. customthe solvent is removed
  5. customthe residue crystallized from 90% methanol

Quellen und Nachweise

ORD-Eintrag
ord-43061dc747784bc193762ab76e125369
Quelldatensatz
uspto-grants-1990_11
Patentnummer
US04968819

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