HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 2868979, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-(2-fluoro-4-nitrophenyl)piperazine | HCID 2783066 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 2868979 | HCID 2868979 | — |
Reaction Steps
A stirred solution of 1-(2-fluoro-4-nitrophenyl)piperazine (15 g, 66.6 mmol) in DCM (160 ml) was cooled to 0° C. Triethylamine was then added (11.23 ml, 79.92 mmol) followed by dropwise addition of acetyl chloride (5.68 ml, 79.92 mmol). The solution was allowed to warm to ambient temperature and stir for 1.5 hour. The reaction mixture was diluted with DCM, washed with water, sat. sodium hydrogen carbonate and brine. It was dried and the solvent was evaporated to give the title compound as a solid which was dried in vac oven overnight at 50° C. (17.46 g, 98%). NMR (400 MHz) 2.05 (s, 3H), 3.30 (dt, 4H, under H2O signal), 3.61 (m, 4H), 7.18 (t, 1H), 8.02 (d, 1H), 8.02 (dd, 1H); m/z 268.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07655652B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-e17ef3292284446c934c45cf16400ca0 |
| Source note | uspto-grants-2010_02 |