HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Bromo-3-chloropropane → HCID 66649121, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Bromo-3-chloropropane | HCID 8006 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 136342633 | HCID 136342633 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66649121 | HCID 66649121 | 62.2% |
Reaction Steps
To a stirred solution of 332 (140 mg, 0.35 mmol) in anhydrous DMF (5 ml) were added 1-bromo-3-chloropropane (553 mg, 3.51 mmol) and cesium carbonate (573 mg, 1.76 mmol), respectively. The reaction mixture was stirred for 2 hrs at room temperature, diluted with AcOEt, and successively washed with water, sat. ammonium chloride, water, and concentrated. The crude material was adsorbed on silica gel and purified by flash column chromatography (eluents AcOEt/CH2Cl2: 10/90 to 20/80) to afford title compound 333 (120 mg, 62% yield) as a yellow solid. MS (m/z): 551.0 and 553.0 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08093264B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-ca68b3211b2342b195fa6b35704e9da1 |
| Source note | uspto-grants-2012_01 |