HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 86760400, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Phenacyl bromide | HCID 6259 | — |
| Reactant | HCID 23716541 | HCID 23716541 | — |
| Solvent | Hexane | HCID 8058 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86760400 | HCID 86760400 | 27% |
Reaction Steps
A solution of sodium 5-(4-fluorophenylcarbamoyl)pyrimidine-2-sulfinate (76 mg, 0.24 mmol) in 2 mL of DMF was treated with 2-bromoacetophenone (48 mg, 0.24 mmol) and stirred at ambient temperature for 3 days. The solution was then diluted with 15 mL ethyl acetate and 5 mL hexane and sequentially washed with 2×5 mL portions of 0.1 M HCl and 5 mL of water. The organic phase was dried using Na2SO4, concentrated and the resultant oil chromatographed through SiO2 (2–5% MeOH/dichloromethane). Recrystallization in ethyl acetate/hexane yielded 26 mg (27%) of the titled compound as yellowish needles. ApcI-MS m/z 414 (MH+), 412 (M−H−).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07176310B1 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-ddfe8006141c42c991d85ef48d5e2f32 |
| Source note | uspto-grants-2007_02 |