HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 15315836, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2-Cyclopenten-1-one | HCID 13588 | — |
| Reactant | Trimethylsilyl triflate | HCID 65367 | — |
| Reactant | Diethylphosphite | HCID 3780918 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15315836 | HCID 15315836 | — |
Reaction Steps
0.52 mmol trimethylsilyltriflate are added dropwise to 11.4 mmol diethylphosphite and 12.4 mmol N,O-bis-(trimethylsilyl)acetamid in 5 ml dichlormethane at 0° C. After 30 minutes of stirring 0.52 mmol 2-cyclopenten-1-one are added dropwise thereto at the same temperature and stirring is continued for 1 h. The enolsilane intermediate product is hydrolized by 3 ml 1 n HCl and 3 hours of stirring. The organic phase is separated, dried over magnesiumsulfate and concentrated. The raw product may be chromatographed on SiO2 and, after concentrating the desired fractions, results to 3-(phosphonic acid diethylester)-cyclopentan-1-one (a) with boiling point0.25 Torr=104° C. in a good yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06753324B2 |
| Source dataset | uspto-grants-2004_06 |
| ORD ID | ord-76a7688b28e34de48d9b84dbe196c58b |
| Source note | uspto-grants-2004_06 |