HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylcarbamoyl Chloride → HCID 69677555, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 18403905 | HCID 18403905 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Acetonitrile methylene chloride | HCID 21877088 | — |
| Product | HCID 69677555 | HCID 69677555 | 73% |
Reaction Steps
To a solution of 2-methoxy-4-[2-(4-pyridin-2-yl-piperazin-1-yl)ethyl)phenol (1.0 g) and cesium carbonate (1.0 g) in 25% acetonitrile/dichloromethane was added dimethylcarbamyl chloride (0.7 g), and the reaction mixture was stirred for 18 hrs, under nitrogen. The reaction mixture was diluted with ethyl acetate, and washed with brine, dried over anhydrous sodium sulfate, and concentrated. The residue was flash chromatographed (silica) eluting with 2% methanol/dichloromethane. The appropriate fractions were collected and concentrated. The residue was dissolved in ethyl acetate and ethereal hydrogen chloride was added. The precipitate was collected to give product 0.9 g (73%), mp 192-193° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06479495B1 |
| Source dataset | uspto-grants-2002_11 |
| ORD ID | ord-80938551bd3a4f71a1d26060724ea38b |
| Source note | uspto-grants-2002_11 |