HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → Benzenesulfonyl chloride, 4-chloro-3-nitro-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Dimethylacetamide | HCID 31374 | — |
| Reactant | Benzenesulfonic acid, 4-chloro-3-nitro-, potassium salt | HCID 81181 | — |
| Solvent | Water | HCID 962 | — |
| Product | Benzenesulfonyl chloride, 4-chloro-3-nitro- | HCID 7323 | 84% |
Reaction Steps
To a mixed solution consisting of 1,280 g of potassium 4-chloro-3 nitrobenzenesulfonate, 1,150 ml of acetonitrile, 250 ml of sulforan, and 30 ml of dimethylacetamide, was added dropwise 1,250 ml of phosphorous oxychloride, while maintaining the inner temperature between 60° C. and 70° C. The mixture was allowed to react at 73° C. for 3 hours. After allowing to cool, 400 ml of water was slowly added thereto, and the reaction mixture was poured into 5l of ice-water. The crystals thus precipitated were filtered, washed with water, and dried to obtain 1,060 g (84%) of the noted compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05071729 |
| Source dataset | uspto-grants-1991_12 |
| ORD ID | ord-b870061e36bc4173a835dcba868b16d0 |
| Source note | uspto-grants-1991_12 |