HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9905971, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 3-Chlorothiophene | HCID 87017 | — |
| Reactant | HCID 22116138 | HCID 22116138 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 9905971 | HCID 9905971 | 30% |
Reaction Steps
This compound is prepared from 2-amino-4-chloro-6-[2-(pyridin-2-yl)ethyl]phenol, and 3-thienyl chloride using method A with 1,4-dioxan as solvent to give the crude amide in a 100% yield. This is treated with methanesulphonic acid in toluene at reflux, with azeotropic removal of water. Purification by flash chromatography (SiO2, EtOAc:hexanes 1:1), gave the title compound, (30%) as a white crystalline solid, m.p. 126-127° C. TLC (SiO2, EtOAc:hexanes 1:1, Rf=0.46). CI Mass Spectrum (methane), m/z=341 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06166041 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-1b5db37a9e1041fb93f0dcb9d1bcd0c5 |
| Source note | uspto-grants-2000_12 |