HRID1633835

反应详情

EQUATION

反应方程式

HRID 1633835 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

66.9 g of 2,4,6-tri-t-butylphenol was dissolved or dispersed into 213.5 g of tri-n-propyl amin. To this solution was added 13.5 of sodium methoxide. The mixture was heated in flask until reflux occurred at about 150° C. When the reflux temperature dropped below 150° C., distillate was condensed and removed from the reaction mixture until the vapor temperature in the flask rose above 150° C. then the mixture was again refluxed. When the vapor temperature dropped below 150° C., distillate was condensed and removed from the reaction mixture until the vapor temperature rose above 150° C. This alternate process of reflux and condensation was repeated until 8.0 g of methyl alcohol, CH3OH had been distilled Away from the reaction mixture. Approximately 112 g of tri-n-propyl amine was stripped from the reaction mixture leaving about 71 g of sodium 2,4,6-tri-t-butyl phenolate in about 100 g of tri-n-propyl amine as a 40 weight percent slurry of the phenolate salt in the amine solvent.

WORKUP

后处理

  1. temperatureThe mixture was heated in flask
  2. temperatureuntil reflux
  3. customoccurred at about 150° C
  4. additionWhen the reflux temperature dropped below 150° C.
  5. customcondensed
  6. customremoved from the reaction mixture until the vapor temperature in the flask
  7. customrose above 150° C.
  8. temperaturethe mixture was again refluxed
  9. additionWhen the vapor temperature dropped below 150° C.
  10. customcondensed
  11. customremoved from the reaction mixture until the vapor temperature
  12. customrose above 150° C
  13. temperatureThis alternate process of reflux
  14. customcondensation
  15. distillationhad been distilled Away from the reaction mixture