反应详情

温度

60 °C

Estolides prepared according to the method set forth in Example 1 (20 mol) and a second-generation Grubbs' catalyst (e.g., C827, 25 ppm) are added to a Parr Reactor and degassed with argon for 1 hr. 1-Butene is added while heating to 60° C. while keeping the pressure of the reaction between about 25 to about 60 psi. The 1-butene is added using a one-way check valve to prevent backflow into the 1-butene cylinder. After 4 hrs, the pressure is released and vented into the fume hood. After allowing the reactor to cool to room temperature, a 50 ml 1M tris-hydroxymethylphopshine (THMP) solution in isopropanol (IPA) (50 mol equiv.) is added, and the reactor is degassed with argon and heated to 60° C. for 18 hrs. The reactor is then again allowed to cool to room temperature. The crude reaction product is then washed with water and brine. The washed reaction product is them dried over sodium sulfate, filtered, and distilled to provide 1-decene, 3-dodecene, estolides having a C10 cap with a terminal double bond, and estolides having a C12 cap with an internal double bond.

1. customEstolides prepared
2. customdegassed with argon for 1 hr
3. addition1-Butene is added
4. customthe pressure of the reaction between about 25 to about 60 psi
5. temperatureto cool to room temperature
6. customthe reactor is degassed with argon
7. temperatureheated to 60° C. for 18 hrs
8. temperatureto cool to room temperature
9. customThe crude reaction product
10. washis then washed with water and brine
11. customThe washed reaction product
12. dry with materialdried over sodium sulfate
13. filtrationfiltered
14. distillationdistilled