HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 69209744, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Malononitrile | HCID 8010 | — |
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | 2-Hydroxy-1-(4-methoxyphenyl)ethanone | HCID 77786 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 69209744 | HCID 69209744 | 87% |
Reaction Steps
To a cooled solution of 2-hydroxy-4′-methoxyacetophenone (379 mg, 2.28 mmol) in DMF (0.75 ml) was added malononitrile (166 mg, 2.51 mmol) followed by diethylamine (0.1 ml, 0.97 mmol). The mixture was stirred at room temperature for 2 hours, and then poured into large amount of cold water. The precipitate was filtrated, washed with water, and dried under reduced pressure to give the intermediate of Example 1(A) (424 mg, 87%) as a brown solid. 1H NMR (400 MHz, CDCl3) ppm 3.83 (s, 3H), 4.73 (brs, 2H), 6.93 (m, 2H), 6.94 (s, 1H), 7.49 (m, 2H). LC/MS: m/z 215 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07427623B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-55958ad6e27d49fa96299ad996a65ea7 |
| Source note | uspto-grants-2008_09 |