HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68776944, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,2,2-Trichloroethyl pyridin-3-ylcarbamate | HCID 68575380 | — |
| Reactant | 1-[3-(Thiophen-2-yl)-1,2,4-thiadiazol-5-yl]piperazine | HCID 68778015 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 68776944 | HCID 68776944 | 37.1% |
Reaction Steps
A mixed solution of 2,2,2-trichloroethyl pyridin-3-ylcarbamate (235 mg, 0.872 mmol), 1-[3-(2-thienyl)-1,2,4-thiadiazol-5-yl]piperazine (200 mg, 0.793 mmol) and diisopropylethylamine (0.152 ml, 0.872 mmol) in dimethyl sulfoxide (2.5 ml) was stirred at 80° C. for 3 hours. Water was poured to the reaction mixture, and the resulting solution was extracted with ethyl acetate. The extract was washed with water, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) and recrystallized from a mixed solvent of hexane and tetrahydrofuran to give 109 mg (37.1%) of the desired product as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07851473B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-17325971e4644a15a710db0b7f31361b |
| Source note | uspto-grants-2010_12 |