HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoromethanesulfonic acid → HCID 45100641, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoromethanesulfonic acid | HCID 62406 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | HCID 18637647 | HCID 18637647 | — |
| Reactant | HCID 86743737 | HCID 86743737 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 45100641 | HCID 45100641 | 96.5% |
Reaction Steps
800 mg of 3β-methyl-16β-trifluoromethylsulfonyloxy-5-androsten-17-one, prepared from 3β-methyl-16α-hydroxy-5-androsten-17-one and trifluoromethane sulfonic acid was placed in 16 ml DMF and was treated with 100 mg Lithium chloride at room temperature. The reaction mixture was stirred magnetically for 21 hours. Water is then added and the resulting crystalline ppt was collected. The crystals were washed with additional water and were then dissolved in CH2Cl2, filtered through anhydrous sodium sulfate and the solvent was evaporated off. The resulting crystals were recrystallized from CH3OH, yielding 570 mg of final product. m.p. 159°-165° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05714481 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-850d024d96b34fc1ba80cdec131913b1 |
| Source note | uspto-grants-1998_02 |