HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyclohexanone → HCID 67865375, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyclohexanone | HCID 7967 | — |
| Reactant | Aluminum isopropoxide | HCID 11143 | — |
| Reactant | Potassium sodium tartarate | HCID 9855836 | — |
| Reactant | HCID 67865743 | HCID 67865743 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67865375 | HCID 67865375 | 66.6% |
Reaction Steps
623 mg (E)-3-fluoromethylene-4-androsten-17-beta-ol is dissolved in 25 ml of toluene, mixed with 7 ml of cyclohexanone and three times with 300 mg of aluminum triisopropylate at 160° C. bath temperature on a water separator. After cooling, it is stirred with potassium sodium tartrate for 30 minutes at 60° C., diluted with dichloromethane, washed neutral, dried on sodium sulfate and concentrated. After chromatography on silica gel with hexane/ethyl acetate, 412 mg (E)-3-fluoromethylene-4-androsten-17-one with a melting point of 142°-143° C. is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04925834 |
| Source dataset | uspto-grants-1990_05 |
| ORD ID | ord-9663b068ff9f480d87c899a020cdf6d7 |
| Source note | uspto-grants-1990_05 |