HuagongsheHuagongshe Chemistry Print Report · For research reference only
methyl 1H-pyrrole-3-carboxylate → Methyl 5-(2,4-Dichlorophenylthio)pyrrole-3-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | methyl 1H-pyrrole-3-carboxylate | HCID 12361759 | — |
| Reactant | 2,4-Dichlorobenzenesulfenyl chloride | HCID 12878542 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 5-(2,4-Dichlorophenylthio)pyrrole-3-carboxylate | HCID 20401058 | — |
Reaction Steps
Under nitrogen, methyl pyrrole-3-carboxylate (3.75 g.) was dissolved in 100 ml. of methylene chloride and cooled in an ice-water bath. To the cold, stirred solution, 2,4-dichlorobenzenesulfenyl chloride (6.39 g., 30 mmoles) was added dropwise. The bath was removed and the reaction stirred at room temperature for 1 hour. An equal volume of ether was added, the mixture filtered and the filtrate evaporated in vacuo to crude product (9.0 g., oil). The oil was chromatographed on 300 g. of silica gel with 200 ml. fractions of the ethyl acetate-1/hexane-7 eluant collected. Fractions 6 to 10 were combined and evaporated to yield purified methyl 5-(2,4-dichlorophenylthio)pyrrole-3-carboxylate (3.7 g., solid, m/e 302).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04282242 |
| Source dataset | uspto-grants-1981_08 |
| ORD ID | ord-58f1a0e2627d41aaac54300932cb7d5a |
| Source note | uspto-grants-1981_08 |