反应详情

A solution of N-methylethylenediamine (27.0 g, 364 mmol) and ethyl trifluoroacetate (96.6 mL, 812 mmol) in a mixture of ACN (350 mL) and water (7.8 mL, 436 mmol) was refluxed with stirring overnight. Solvents were evaporated in vacuo. The residue was re-evaporated with i-PrOH (3×100 mL), followed by heat-cool crystallization from DCM (500 mL). Formed crystals were filtered, washed with DCM and dried in vacuo to provide compound A (88.3 g, 85%) as white solid powder.

1. temperaturewas refluxed
2. customSolvents were evaporated in vacuo
3. customThe residue was re-evaporated with i-PrOH (3×100 mL)
4. temperatureby heat-cool
5. customcrystallization from DCM (500 mL)
6. customFormed crystals
7. filtrationwere filtered
8. washwashed with DCM
9. customdried in vacuo