HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus pentachloride → HCID 59562500, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus pentachloride | HCID 24819 | — |
| Reactant | HCID 67524030 | HCID 67524030 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 59562500 | HCID 59562500 | 82.9% |
Reaction Steps
To a solution of 1-methyl-8-oxa-bicyclo[3.2.1]octane-2,4-dione (175 mg, 1.14 mmol) in chloroform (2 ml) is added, under N2, in one portion, the phosphorous pentachloride (135 mg, 0.65 mmol). The reaction mixture is stirred for reflux for 5 hours. Silica gel is added to the cooled crude reaction mixture, the solvent is evaporated under reduced pressure and the residue is purified by flash chromatography on silica gel to give 4-chloro-1-methyl-8-oxa-bicyclo[3.2.1]oct-3-en-2-one (93 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08956999B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-f973f5cfddb34566a345528007034731 |
| Source note | uspto-grants-2015_02 |