HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → Diethyl 2-acetylaminoethylphosphonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Diethyl (2-aminoethyl)phosphonate | HCID 2733596 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | Diethyl 2-acetylaminoethylphosphonate | HCID 23263408 | 93.5% |
Reaction Steps
To a solution of diethyl 2-aminoethylphosphonate (10.5 g), triethylamine (7.0 g) in dichloromethane (200 ml) at 0° C. was added dropwise acetic anhydride (7.1 g). After 20 hours at room temperature, the reaction mixture was diluted with brine, made basic with 5% aqueous potassium carbonate, and extracted twice with dichloromethane. The extract was dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel (5% methanol in chloroform) to give (12.1 g) of diethyl 2-acetylaminoethylphosphonate as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05495023 |
| Source dataset | uspto-grants-1996_02 |
| ORD ID | ord-df32361a083e44c8b73a3365e6fc906c |
| Source note | uspto-grants-1996_02 |