反应详情

温度

260 °C

Compound 6B (2000 g, 5.468 mol) was introduced into the reactor. Dowtherm (4.000 L) was charged to the reactor and degassed at room temperature overnight with nitrogen purge. It was then stirred and warmed to 260° C. EtOH produced was distilled off. The reaction was monitored and was complete after 5.5 h, the reaction was substantially complete. Heat source was removed and the reaction mixture was cooled to 80° C. and heptane (2.000 L) was charged. The mixture was stirred for 30 min. Heptane (6.000 L) was charged to the stirred mixture and stirring continued overnight. Solids were filtered off and washed with heptane (4.000 L) and dried in a vacuum oven at 50° C. to provide Compound 6A.

1. customdegassed at room temperature overnight with nitrogen
2. custompurge
3. customEtOH produced
4. distillationwas distilled off
5. temperatureHeat source
6. customwas removed
7. temperaturethe reaction mixture was cooled to 80° C.
8. additionheptane (2.000 L) was charged
9. stirringThe mixture was stirred for 30 min
10. additionHeptane (6.000 L) was charged to the stirred mixture
11. stirringstirring continued overnight
12. filtrationSolids were filtered off
13. washwashed with heptane (4.000 L)
14. customdried in a vacuum oven at 50° C.