Tripropylamine → 27801-58-7

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.

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

ORDレコード

ord-0c029dc401a44020a8e149dbcc63d0a2

出典データセット

uspto-grants-2003_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06504065B1