HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 11508866, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1-(4-Phenyl-1,3-thiazol-2-yl)piperazine | HCID 712468 | — |
| Reactant | HCID 86625475 | HCID 86625475 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 11508866 | HCID 11508866 | 27.8% |
Reaction Steps
A mixed solution of bis(2,2,2-trichloroethyl)pyridin-3-ylimidodicarbonate (359 mg, 0.810 mmol), 1-(4-phenyl-1,3-thiazol-2-yl)piperazine (396 mg, 1.62 mmol) and diisopropylethylamine (0.281 ml, 1.62 mmol) in dimethyl sulfoxide (2.7 ml) was stirred at 70° 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 dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (100% ethyl acetate) and recrystallized from a mixed solvent of hexane and tetrahydrofuran to give 82.0 mg (27.8%) of the desired product as a solid. mp 74-75° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07851473B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-95e5a8d44e0149fba1464ed0223be0a4 |
| Source note | uspto-grants-2010_12 |