HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfate → HCID 13322356, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | N-(4-Chlorophenyl)-4-[(dimethylsulfamoyl)amino]benzamide | HCID 13322327 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 13322356 | HCID 13322356 | 96.2% |
Reaction Steps
A mixture of 300 mg of 4'-chloro-4-[(dimethylaminosulfonyl)amino]benzanilide 7, 140 mg of potassium carbonate, 130 mg of dimethyl sulfate 8, and 10 ml of dried acetone is refluxed for 30 minutes. Acetone is distilled off from the reaction mixture, the residue is basified with 10% sodium hydroxide solution and extracted with methylene chloride. The organic layer is washed with water, dried over anhydrous sodium sulfate, and concentrated. The residue is crystallized from ethyl acetate-isopropyl ether to give 300 mg of 4'-chloro-4-[methyl(dimethylaminosulfonyl)amino]benzanilide 9 as crystals, m.p. 155°-156° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04595780 |
| Source dataset | uspto-grants-1986_06 |
| ORD ID | ord-1c369b3d02594e71adb41949ae25eb86 |
| Source note | uspto-grants-1986_06 |