HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 90014067, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Chlorobutyronitrile | HCID 12336 | — |
| Reactant | HCID 54204764 | HCID 54204764 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 90014067 | HCID 90014067 | 69% |
Reaction Conditions
| Temperature | -10 °C |
|---|
Reaction Steps
The mixture of diethyl 2-(2-hydroxyethylamino)ethylphosphonate (6 g, 26.7 mmol) and K2CO3 (3.7 g, 26.7 mmol) in dry acetonitrile (80 ml) was cooled to −10° C. and 4-chlorobutyronitrile (4.16 g, 40 mmol) was added. The reaction mixture was stirred at −10° C. for 1 h and then heated at 80° C. for 70 h. The solvent was then removed by evaporatation. Water and CHCl3 were added, the organic layer separated, washed with brine and dried over anhydrous MgSO4. After filtration, solvent was evaporated and the residue was purified by column chromatography on silica gel (CHCl3-MeOH), the diethyl 2-(2-cyanopropylamino)ethylphosphonate was obtained in 69% yield (5.38 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09200020B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-e9f47743305847eab5c4a663c4c31244 |
| Source note | uspto-grants-2015_12 |