Reaktion #331550

Reaktionsgleichung

isopropenyl chloride carbonate

4-nitrophenol

chloroform

→

title compound

Ausbeute 17.6%

Isopropenyl 4-nitrophenyl carbonate

Ausbeute 17.6%

Lösungsmittel

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooling over a period of 20 minutes
2. 2
   Temperaturcooling for 15 minutes
3. 3
   workup.STIRRINGfurther stirred overnight
4. 4
   Waschenthe reaction solution was washed succesively with 1N aqueous hydrochloric acid solution, water
5. 5
   Trocknena satureated aqueous sodium chloride solution, dried over magnesium sulfate
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated
8. 8
   SonstigeThe obtained residue was purified by column chromatography (hexane:ethyl acetate=4:1)

Vorschrift

To isopropenyl chloride carbonate (6.68 g) were added 4-nitrophenol (5 g) and chloroform (150 ml), and thereto was added drowpise pyridine (2.9 ml) under ice-cooling over a period of 20 minutes. Then, the mixture was stirred under ice-cooling for 15 minutes, then warmed to room temperature, and further stirred overnight. After the reaction was completed, the reaction solution was washed succesively with 1N aqueous hydrochloric acid solution, water and a satureated aqueous sodium chloride solution, dried over magnesium sulfate, filtered and concentrated. The obtained residue was purified by column chromatography (hexane:ethyl acetate=4:1) to give the title compound (1.41 g).

Quelle