HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 57879640, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 19076692 | HCID 19076692 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 57879640 | HCID 57879640 | 90% |
Reaction Steps
A 1 L four-neck flask equipped with a stirrer, a thermometer and a condenser tube was charged with 82.6 g (0.5 mol) of 7-methyl-1,2-benzisothiazol-3-one, 80.4 g (1.1 mol) of N,N-dimethylformamide and 200.0 g of toluene. While stirring, 83.3 g (0.7 mol) of thionyl chloride was added dropwise thereto at 70° to 80° C. over 1 hour, and the mixture was reacted at the same temperature for 3 hours. After terminating the reaction, the liquid reaction mixture was concentrated, and a crude product obtained was distillated under reduced pressure of 0.40 kPa at 110° C. to give 81.7 g (0.45 mol) of 3-chloro-7-methyl-1,2-benzisothiazole. The yield based on 7-methyl-1,2-benzisothiazol-3-one was 89%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08664404B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-add80d5cd62f4eb9ae0b55fbc71c6407 |
| Source note | uspto-grants-2014_03 |