Reaktion #83835

Reaktionsgleichung

phosphate

2-Methyl-4,5-dihydrofuran

mercaptoacetic acid

p-toluenesulfonic acid mono-hydrate

→

26

2-Carboxymethylthio-2-methyltetrahydrofuran

Lösungsmittel

water

ethyl acetate

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis cooled
2. 2
   Temperaturis maintained between -10° C. to -25° C
3. 3
   Sonstigeto come to room temperature
4. 4
   SonstigeOrganic layer is separated
5. 5
   Extraktionthe aqueous layer is extracted with ethyl acetate
6. 6
   TrocknenThe combined ethyl acetate layer is dried
7. 7
   Sonstigeevaporated

Vorschrift

A solution of mercaptoacetic acid (10 mmol) in 5 mL of dichloromethane containing p-toluenesulfonic acid mono-hydrate (100 mg) is cooled with stirring to -10° to -25° C. 2-Methyl-4,5-dihydrofuran (10 mmol) in 10 mL of dichloromethane is added dropwise to the cold solution while the temperature is maintained between -10° C. to -25° C. Then 5 mL of phosphate buffer is added and the solution is allowed to come to room temperature. The mixture is poured into a 30 mL of ethyl acetate and 10 mL of water. Organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined ethyl acetate layer is dried and evaporated to give 26 as a colorless oil.

Quelle