HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9949854, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 2-Chlorothiophene | HCID 7299 | — |
| Reactant | HCID 22116138 | HCID 22116138 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 9949854 | HCID 9949854 | 31% |
Reaction Steps
This compound is prepared from 2-amino-4-chloro-6-[2-(pyridin-2-yl)ethyl]phenol and 2-thienyl chloride using method A, with ethyl acetate as solvent to give the crude amide in 99% yield. This is treated with methanesulphonic acid in toluene at reflux, with azeotropic removal of water to give the title compound, (31%) as a white crystalline solid after trituration and recrystallisation (EtOAc), m.p. 90-91° C. TLC (SiO2 ; EtOAc:hexanes 1:1, Rf=0.46). Mass Spectrum CI (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-1047d4d4c87040f5823e4e4f8f9b3391 |
| Source note | uspto-grants-2000_12 |