HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68778443, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | tert-Butyl 4-carbamothioylpiperidine-1-carboxylate | HCID 2735648 | — |
| Reactant | 2-Bromo-2'-fluoroacetophenone | HCID 2737449 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68778443 | HCID 68778443 | 26.4% |
Reaction Steps
A solution of 2-bromo-1-(2-fluorophenyl)ethanone (977 mg, 4.50 mmol), tert-butyl 4-(aminocarbonothioyl)piperidine-1-carboxylate (1.0 g, 4.09 mmol) and potassium carbonate (1.13 g, 8.18 mmol) in dimethylformamide (30 ml) was stirred at 110° C. for 1 hour. Water was poured into the reaction solution, and the mixture 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 (hexane:ethyl acetate=9:1) to give the desired product (391 mg, 26.3%) as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07851473B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-f2fb521eb9624cd9916d81f666aae433 |
| Source note | uspto-grants-2010_12 |