HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 70565434, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Chlorine | HCID 24526 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 14823699 | HCID 14823699 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 70565434 | HCID 70565434 | — |
Reaction Steps
To a solution of 9-fluoro-11β-hydroxy-17-(methylthio)androsta-1,4,16-trien-3-one (100 mg) in a mixture of dry dichloromethane (10 ml) and methanol (8 ml) is added a 0.31 molar solution of chlorine in dichloromethane (1.0 ml). After a few hours, the solution is poured into a dilute sodium bicarbonate solution. The product is isolated by extraction with chloroform and the chloroform solution is washed with water, dried (anhydrous MgSO4) evaporated and the residue is purified by preparative thin layer chromatography to afford the title compound (35 mg), melting point 262°-268° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04265815 |
| Source dataset | uspto-grants-1981_05 |
| ORD ID | ord-3b55fee2c5764235b67c3b9183a9df2c |
| Source note | uspto-grants-1981_05 |