Reaktion #93852

Reaktionsgleichung

water

methyl 2,2-dimethyl-4-(p-methoxyphenyl)-3-(p-toluenesulphonamido)butyrate

sodium hydride

methyl iodide

→

Methyl 2,2-dimethyl-4-(p-methoxyphenyl)-3-(N-methyl-p-toluenesulphonamido)butyrate

Ausbeute 96.0%

Lösungsmittel

—

same solvent

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONis added
2. 2
   TemperaturAfter an additional period of heating
3. 3
   Temperatur(under reflux) the mixture
4. 4
   Temperaturafter being cooled
5. 5
   FiltrationAfter filtration
6. 6
   Sonstigedrying it melts at 132°-134° C

Vorschrift

A solution of 405 g of methyl 2,2-dimethyl-4-(p-methoxyphenyl)-3-(p-toluenesulphonamido)butyrate in 1800 ml of dry dimethylformamide is added to a mechanically stirred suspension of 52.8 g of sodium hydride in 320 ml of the same solvent. After the reaction mixture has been heated at 80° C. for 1 hour it is cooled when 93 ml of methyl iodide is added. After an additional period of heating (under reflux) the mixture, after being cooled, is poured into plenty of water. A white crystallisate separates. After filtration and drying it melts at 132°-134° C. Yield 96%.

Quelle