HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Bromobenzenesulfonyl chloride → HCID 57282319, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Bromobenzenesulfonyl chloride | HCID 7396 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 21-Hydroxy-16α-methylpregna-1,4,9(11)-triene-3,20-dione | HCID 14585239 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 57282319 | HCID 57282319 | 67.07% |
Reaction Steps
To a solution containing 10.0 g (29.4 moles) of 21-hydroxy-16α-methylpregna-1,4,9(11)-triene-3,20-dione in 100 mol of tetrahydrofuran, first 7,14 ml (51.4 mmoles) of triethylamine, then at 0° C. 13.1 g (51.4 moles) of 4-bromobenzenesulfonyl chloride are added, the reaction mixture is stirred at room temperature for 4 hours, then it is dropwise added to 450 ml of water while stirring. The precipitate is filtered off, dried and recrystallized from ether to obtain 11.0 g (67.07%) of the title compound, m.p.: 124°-129° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05550240 |
| Source dataset | uspto-grants-1996_08 |
| ORD ID | ord-a2b276ca76e24203b3e38a4925daf82a |
| Source note | uspto-grants-1996_08 |