HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 11796154, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | HCID 10667564 | HCID 10667564 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 11796154 | HCID 11796154 | 41.7% |
Reaction Steps
To a stirred solution of 2-ethoxycarbonyl-2-(2-trichloroacetylpyrrol-1-yl)succinimide (6.0 g) in chloroform (50 ml) was added dropwise a solution of sulfuryl chloride (4.8 g) in chloroform (5 ml) under ice cooling. The resulting mixture was stirred under ice cooling for 30 minutes, poured into water, and extracted with chloroform. The extracts were dried over sodium sulfate and concentrated under reduced pressure. The residue was chromatographed on silica gel using n-hexane/ethyl acetate (2:1) as the eluent. Fractions containing the title compound were pooled and evaporated under reduced pressure. The residue was recrystallized from ethyl acetate/n-hexane to give the title compound (2.5 g, 41.7%) as colorless crystals, mp 182°-185° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05258382 |
| Source dataset | uspto-grants-1993_11 |
| ORD ID | ord-75c3a3072c33450d9948e44858a1376b |
| Source note | uspto-grants-1993_11 |