HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 15315828, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2-Cyclohexen-1-one | HCID 13594 | — |
| Reactant | Trimethylsilyl triflate | HCID 65367 | — |
| Reactant | Diethylphosphite | HCID 3780918 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15315828 | HCID 15315828 | 95% |
Reaction Steps
0.52 mmol trimethylsilyltriflate is added dropwise to 11.4 mmol diethylphosphite and 12.4 mmol N,O-bis-(trimethylsilyl)acetamide in 5 ml dichlormethane at 0° C. After 30 minutes of stirring at the same temperature 0.52 mmol 2-cyclohexen-1-one are added dropwise thereto and is stirred for 1 h. The enolsilane intermediate product is hydrolized by 3 ml 1 n HCl during 3 hours of stirring. The organic phase is separated, dried over magnesiumsulfate and concentrated. The raw product can be chromatographed on SiO2 and after concentration of the desired fractions results in 3-oxo-cyclohexylphosphonic acid diethylester 2(a) in a 95% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06753324B2 |
| Source dataset | uspto-grants-2004_06 |
| ORD ID | ord-884ec04ad3304fed892541bf755c009a |
| Source note | uspto-grants-2004_06 |