HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Benzenesulfonyl chloride, 4-chloro-3-nitro-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Benzenesulfonic acid, 4-chloro-3-nitro-, potassium salt | HCID 81181 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Sulfolane | HCID 31347 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | Benzenesulfonyl chloride, 4-chloro-3-nitro- | HCID 7323 | — |
Reaction Steps
To a solution mixture of 1,280 g of potassium 4-chloro-3-nitrobenzenesulfonate in 1,150 ml of acetonitrile, 250 ml of sulfolane and 30 ml of dimethylacetamide was added dropwise 1,250 ml of phosphorus oxychloride while the temperature was kept at 60° to 70° C. After the reaction proceeded for 3 hours at 73° C., the reaction mixture was cooled with water, then 400 ml of water was added thereto gradually, and then 5 liters of ice water was poured into the reaction mixture. The deposited crystals were filtered followed by washing with water and drying.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04939066 |
| Source dataset | uspto-grants-1990_07 |
| ORD ID | ord-9081fd0728b34433930572bc9c05281c |
| Source note | uspto-grants-1990_07 |