HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diazald → 3-Methoxy-2-(2,4-dichlorobenzoyl)cyclohex-2-enone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diazald | HCID 6628 | — |
| Reactant | Diazomethane | HCID 9550 | — |
| Reactant | 2-(2,4-Dichlorobenzoyl)cyclohexane-1,3-dione | HCID 14301621 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 3-Methoxy-2-(2,4-dichlorobenzoyl)cyclohex-2-enone | HCID 14796556 | 35% |
Reaction Steps
2-(2,4-Dichlorobenzoyl)cyclohexane-1,3-dione (2.85 g, 0.01 ml) was stirred as a suspension in 25 ml anhydrous ether. Diazomethane, generated from Diazald™ (50 ml, 0.02 mol) was added at 0° at a rate slow enough to control effervescence. The resulting solution was stirred for an hour and the solvent allowed to evaporated under a stream of nitrogen in a beaker. The resulting oil was dissolved in ether and washed twice with saturated aqueous K2CO3. Evaporation of the solvent under reduced pressure yielded a solid (1.0 g, 35%, m.p. 81°-86° C.), the nuclear magnetic, infrared and mass spectra of which were consistent with the structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04957540 |
| Source dataset | uspto-grants-1990_09 |
| ORD ID | ord-34697cee103247a9a28655054ec443e7 |
| Source note | uspto-grants-1990_09 |