HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 53687753, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Cyclobutanecarbonyl chloride | HCID 78705 | — |
| Reactant | HCID 22823472 | HCID 22823472 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 53687753 | HCID 53687753 | 96% |
Reaction Steps
To a mixture of 2 g (7.37 mmol) 4-methoxymorphinan-6-one (H2O was removed azeotropic) and 3 g (21.71 mmol) K2CO3 in 20 ml dry DMF was dropped at room temperature during 15 min. a solution of 900 mg (7.59 mmol) cyclobutanecarboxylic acid chloride. This mixture was stirred at room temperature for 1 h, then poured on 200 ml ice water and extracted with ether. The organic layer was extracted with 2 N HCl and brine, dried and evaporated to give an oil, which was crystallized with benzene/u/hexane to yield 2.5 g (96%) N-cyclobutylcarbonyl-4-methoxymorphinan-6-one, m.p. 125°-126°, [α]D26 -204.5° (c 0.76, CHCl3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04388463 |
| Source dataset | uspto-grants-1983_06 |
| ORD ID | ord-ec3d7d4df4354824b34b0070c661bd75 |
| Source note | uspto-grants-1983_06 |