反应详情

IMS (2.5 L, 10 vol) was added to the dichloromethane solution from step (i) above. The solution was distilled until the internal temperature reached 70° C. Approximately 1250 mL of solvent was collected. More IMS (2.5 L, 10 vol) was added followed by benzylamine (120 mL, 0.7 eq.) in one portion (no exotherm seen), and the reaction was heated at reflux for 6 hours (no change from 2 hour sampling point). More benzylamine was added (15 mL) and the solution was heated for a further 2 hours. The IMS was distilled off (ca. 3.25 L) and toluene was added (2.5 L). More solvent was distilled (ca. 2.4 L) and then further toluene added (1 L). The head temperature was now 110° C. A further 250 mL of solvent was collected at 110° C. Theoretically, this left the product in ca. 2.4 L of toluene at 110° C. This solution was used in the next step.

1. distillationThe solution was distilled until the internal temperature
2. customreached 70° C
3. customApproximately 1250 mL of solvent was collected
4. additionMore IMS (2.5 L, 10 vol) was added
5. temperaturewas heated
6. temperatureat reflux for 6 hours (no change from 2 hour
7. aliquotsampling point)
8. temperaturethe solution was heated for a further 2 hours
9. distillationThe IMS was distilled off (ca. 3.25 L) and toluene
10. additionwas added (2.5 L)
11. distillationMore solvent was distilled (ca. 2.4 L)
12. additionfurther toluene added (1 L)
13. customwas now 110° C
14. customA further 250 mL of solvent was collected at 110° C
15. waitTheoretically, this left the product in ca. 2.4 L of toluene at 110° C