Reaktion #446437

Reaktionsgleichung

1-(2,2-dimethyltetralin-1-yl)-5-imidazolecarboxylic acid methyl ester

ammonium peroxodisulfate

sodium hydroxide

→

1-(2,2-dimethyl-4-oxotetralin-1-yl)-5-imidazolecarboxylic acid methyl ester

Ausbeute 28.2%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe suspension is heated to +87° C.
2. 2
   TemperaturAfter the reaction mixture has been cooled to +15° C.
3. 3
   Extraktionthe whole is extracted with 500 ml of methylene chloride
4. 4
   SonstigeThe organic phase is separated off
5. 5
   Trocknendried over sodium sulfate
6. 6
   workup.ADDITIONtreated with activated carbon
7. 7
   Einengenconcentrated by evaporation
8. 8
   SonstigeCrystallisation of the residue from ether

Vorschrift

142 g of 1-(2,2-dimethyltetralin-1-yl)-5-imidazolecarboxylic acid methyl ester are suspended in 1 liter of distilled water. The suspension is heated to +87° C. and, while stirring, a total of 335 g of ammonium peroxodisulfate is added in portions thereto within a period of 1.5 hours in such a manner that the temperature does not exceed +90° C. After the reaction mixture has been cooled to +15° C., the pH value is adjusted to pH 4 by the addition of approximately 335 g of 30% sodium hydroxide solution and the whole is extracted with 500 ml of methylene chloride. The organic phase is separated off, dried over sodium sulfate, treated with activated carbon and concentrated by evaporation. Crystallisation of the residue from ether yields 42 g of 1-(2,2-dimethyl-4-oxotetralin-1-yl)-5-imidazolecarboxylic acid methyl ester having a melting point of 93°-95° C.

Quelle