HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9952370, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Benzo[b]thiophene-2-carbonyl Chloride | HCID 142384 | — |
| Reactant | HCID 22116138 | HCID 22116138 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 9952370 | HCID 9952370 | 41% |
Reaction Steps
This compound is prepared from 2-amino-4-chloro-6-[2-(pyridin-2-yl)ethyl]-phenol and benzo[b]thiophene-2-carbonyl chloride using method A with 1,4-dioxan as solvent to give the crude amide (73%). This is treated with methanesulphonic acid in toluene at reflux with azeotropic removal of water to give the title compound, (41%) as a white crystalline solid m.p.=183-184° C. TLC (SiO2, EtOAc:hexanes 1:1, Rf=0.56). CI Mass Spectrum (methane) m/z=391 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06166041 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-207f9d94bf894bd8b7974625545a2614 |
| Source note | uspto-grants-2000_12 |