Water → HCID 13429029, compound

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

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

ORD record

ord-ff9a444ef4a44c01a3c96331e9cc54a0

Source dataset

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09040032B2