HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuryl chloride → HCID 15351950, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 15351949 | HCID 15351949 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15351950 | HCID 15351950 | — |
Reaction Steps
6 ml of sulphuryl chloride at 10% in dichloromethane is added under an inert atmosphere, at ambient temperature to a solution of 1.08 g of 11β-[4-(2-(dimethylamino)ethoxy)phenyl]-estra-4,9-diene-3,17-dione in 11 ml of pyridine and agitation is carried out for 30 minutes at approximately −36° C. The reaction medium is poured into sodium bicarbonate, followed by extraction, washing, drying and evaporating under reduced pressure until 1.84 g of crude product is obtained, which is purified by chromatography, eluting with an ethyl acetate/triethylamine mixture 80/20. 616 mg of expected pure product is obtained. (Rf AcOEt/TEA 8/2=0.35).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06239121B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-6889b676106b4e9a8a0023ac051ba7f9 |
| Source note | uspto-grants-2001_05 |