HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thionyl Chloride → 2,6,7-Trichloro-benzothiazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | 2(3H)-Benzothiazolethione, 6,7-dichloro- | HCID 178527791 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2,6,7-Trichloro-benzothiazole | HCID 57748854 | 41.9% |
Reaction Steps
To a suspension of 300 mg (1.270 mmol) 6,7-dichloro-benzothiazole-2-thiol in 1.4 mL (19.05 mmol) thionyl chloride was added dropwise 32.3 □L N,N-dimethylformamide dry at room temperature. The mixture was stirred at room temperature for 4 h. The solvent was removed in vacuo. The residue was purified with flash column chromatography on silica eluting with a gradient formed from n-heptane and ethyl acetate to provide 127 mg (41.9%) of the title compound as a yellow solid. MS(m/e): 239 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07897627B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-ffb89a1d559d41edb66e5f362008ee1e |
| Source note | uspto-grants-2011_03 |