反应详情

温度

-10 °C

Charge an inertized reactor with 39.6 g of 1-[(dimethylamino)methyl]-ferrocene and 360 ml of MTBE. Distill about 160 ml of MTBE (4V) at atmospheric pressure. Cool the solution to −10° C. and slowly add 98.2 ml of a solution of t-BuLi in heptane (titer 16%). Stir the reaction mixture at −10° C. for 2 hours and then at 0° C., slowly add 25.2 ml of DMF. Continue stirring the reaction mixture at 20° C. for 2 hours then at 5° C., slowly add 135 ml of 1.5N aqueous HCl. Continue stirring the reaction mixture at 5° C. for 30 min, then at 20° C. for 30 min. Leave the reaction mixture to settle and withdraw the aqueous phase then the MTBE phase. Counter-extract the aqueous phase with 125 ml of MTBE. Filter the combined MTBE phases on activated charcoal then concentrate to 120 ml under vacuum. Add 80 ml of isopropanol then distill 420 ml of solvent to constant volume, under vacuum, by regular addition of isopropanol. At the end of distillation, dilute the reaction mixture to 280 ml with isopropanol. 39.9 g of the expected compound is obtained in solution in isopropanol.

1. distillationDistill about 160 ml of MTBE (4V) at atmospheric pressure
2. customat 0° C.
3. stirringContinue stirring the reaction mixture at 20° C. for 2 hours
4. customat 5° C.
5. stirringContinue stirring the reaction mixture at 5° C. for 30 min
6. waitat 20° C. for 30 min
7. customLeave the reaction mixture
8. customwithdraw the aqueous phase
9. extractionCounter-extract the aqueous phase with 125 ml of MTBE
10. filtrationFilter the combined MTBE phases on activated charcoal
11. concentrationthen concentrate to 120 ml under vacuum
12. additionAdd 80 ml of isopropanol
13. distillationthen distill 420 ml of solvent to constant volume
14. additionunder vacuum, by regular addition of isopropanol
15. distillationAt the end of distillation
16. additiondilute the reaction mixture to 280 ml with isopropanol