HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86738041, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | 6-Hydroxy-1,4,4-trimethylbicyclo[3.2.0]heptane-2,3-dione 3-oxime | HCID 86738042 | — |
| Solvent | Ethylene Glycol | HCID 174 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86738041 | HCID 86738041 | 50.9% |
Reaction Steps
To a solution of 2050 mg of the ketoxime (VI) in 25 ml of ethylene glycol, was added 0.7 ml of 80% hydrazine hydrate. After having been kept at 40° to 50° C. for 30 minutes, the solution was admixed with 750 mg of potassium hydroxide and kept at 150° C. for 4 hours under an argon atmosphere. After cooling and adding 50 ml of water, the solution was neutralized with 1 N HCl and extracted with methylene chloride. The extract was washed with an aqueous sodium bicarbonate solution, then with an aqueous sodium chloride solution, dried over magnesium sulfate, and concentrated in vacuo to give 970 mg of a crystalline compound (V). M.p. 130°-133° C.; MS m/e: 183 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04296036 |
| Source dataset | uspto-grants-1981_10 |
| ORD ID | ord-81bdb3c6271f425891d340cff9a63ec4 |
| Source note | uspto-grants-1981_10 |