Reaktion #343932

Reaktionsgleichung

methylene chloride water

4,4'-dihydroxybiphenyl

trimethylamine

propargyl chloroformate

→

title compound

Ausbeute 93.6%

4,4'-Bis(propargyloxycarbonyloxy)biphenyl

Ausbeute 93.6%

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA flask equipped with a stirrer
2. 2
   Temperaturthermometer, nitrogen gas tube and reflux condenser
3. 3
   Sonstigeto react for 6 hours at 30° C
4. 4
   SonstigeAfter the reaction
5. 5
   Sonstigethe organic phase was separated
6. 6
   Trocknenby drying over magnesium sulfate overnight
7. 7
   FiltrationAfter filtering
8. 8
   Sonstigethe filtrate was evaporated in a rotary evaporator
9. 9
   SonstigeThe resulting crystals were recrystallized

Vorschrift

A flask equipped with a stirrer, thermometer, nitrogen gas tube and reflux condenser was charged with 18.6 g of 4,4'-dihydroxybiphenyl and 23.0 g of trimethylamine in 50.0 g of methylene chloride. To the flask was added 26.0 g of propargyl chloroformate dropwise over one hour and the mixture was allowed to react for 6 hours at 30° C. After the reaction, the reaction mixture was treated with methylene chloride-water mixture and the organic phase was separated followed by drying over magnesium sulfate overnight. After filtering, the filtrate was evaporated in a rotary evaporator. The resulting crystals were recrystallized to give the title compound at a yield of 93.6% of theory.

Quelle