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 M (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

ORD record

ord-88c1d202f727447e899d72bd3b6422de

Source dataset

uspto-grants-2014_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08802681B2