HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 3-Chloro-N-(3-chloropropyl)-4-methylaniline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 3-Chloro-4-methylaniline | HCID 7255 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 1-Chloro-3-iodopropane | HCID 81363 | — |
| Solvent | Water | HCID 962 | — |
| Product | 3-Chloro-N-(3-chloropropyl)-4-methylaniline | HCID 11701589 | 61% |
Reaction Steps
A mixture of 3-chloro-4-methylaniline (7.79 g, 55 mmol), 1-chloro-3-iodopropane (5.91 ml, 55 mmol), cesium carbonate (35.84 g, 110 mmol) and DMF (15 ml) was stirred at room temperature for 19 hours. To the mixture was added water (75 ml), and the mixture was extracted with hexane (60 ml, 30 ml×2). The organic layer was washed with water (10 ml), dried over magnesium sulfate and concentrated under reduced pressure. The concentrate was subjected to column chromatography (silica gel 200 g, hexane/ethyl acetate=1/0 to 19/1), and the desired fraction was concentrated under reduced pressure to give the titled compound (7.30 g, 33 mmol, Yield 61%) as a pale brown oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06562978B1 |
| Source dataset | uspto-grants-2003_05 |
| ORD ID | ord-a575456d03614ecb8c839cb8963af4fc |
| Source note | uspto-grants-2003_05 |