Reaktion #343931

ord-3871fff872f44c6e9f669129342353af

Reaktionsgleichung

C#CCOC(=O)Cl
propargyl chloroformate
Oc1ccc(Cc2ccc(O)cc2)cc1
bis(4-hydroxyphenyl)methane
ClCCl
methylene chloride
CN(C)C
trimethylamine
C#CCOC(=O)Oc1ccc(Cc2ccc(OC(=O)OCC#C)cc2)cc1
title compound
Ausbeute 93.6%
C#CCOC(=O)Oc1ccc(Cc2ccc(OC(=O)OCC#C)cc2)cc1
Bis(4-propargyloxycarbonyloxyphenyl)methane
Ausbeute 93.6%

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

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 20.0 g of bis(4-hydroxyphenyl)methane, 50.0 g of methylene chloride and 23.0 g of trimethylamine. 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 melting at 60° C. at a yield of 93.6% of theory.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05258542uspto-grants-1993_11