Water → HCID 13429029, compound

A solution of N-ethylethylenediamine (10.0 g, 113.4 mmol) and ethyl trifluoroacetate (32.0 mL, 261 mmol) in the mixture of acetonitrile (110 mL) and water (2.5 mL, 139 mmol) was refluxed with stirring overnight (˜18 h). Solvents were evaporated in vacuo. Residue was re-evaporated with i-PrOH (3×100 mL). Residue was dissolved in dichloromethane (500 mL) and left overnight at room temperature. The formed crystals were filtered, washed with dichloromethane (100 mL) and dried in vacuo to provide compound JJ (24.6 g, 82.4 mmol) as white solid powder.

1. temperaturewas refluxed
2. customSolvents were evaporated in vacuo
3. customResidue was re-evaporated with i-PrOH (3×100 mL)
4. dissolutionResidue was dissolved in dichloromethane (500 mL)
5. waitleft overnight at room temperature
6. filtrationThe formed crystals were filtered
7. washwashed with dichloromethane (100 mL)
8. customdried in vacuo
9. customto provide compound JJ (24.6 g, 82.4 mmol) as white solid powder

ORD record

ord-575be666538b40488e9d6aac87f8130a

Source dataset

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09040032B2