HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 22119889, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | HCID 15477620 | HCID 15477620 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22119889 | HCID 22119889 | 31.8% |
Reaction Steps
A mixture of 1-methyl-3-(3-methyl-1,2-benzisothiazol-5-yl)-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione (1.00 g, 0.00293 mol), sulfuryl chloride (2.00 g 0.0148 mol) and 1,2-dichloroethane is stirred for five hours at reflux, cooled to room temperature, and diluted with methylene chloride. The resultant mixture is washed with saturated sodium bicarbonate and brine, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to obtain a residue. The residue is chromatographed on silica gel with ethyl acetate/hexanes to afford the title product as a white solid (0.350 g, 31.8%, mp 252-254° C.) which is identified by NMR spectral analysis.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06156700 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-149311686d794393a08f4471b9efeb2f |
| Source note | uspto-grants-2000_12 |