HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 15457070, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Propargyl alcohol | HCID 7859 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 15457065 | HCID 15457065 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 15457070 | HCID 15457070 | 91% |
Reaction Steps
0.04 g (1.10 mmol) of sodium hydride was suspended in 5 ml of DMF, and 0.06 g (1.10 mmol) of propargyl alcohol was dropwise added thereto at room temperature, followed by stirring for 30 minutes. Then, 0.40 g (1.00 mmol) of 3-(4-chloro-2-fluoro-5-bromomethylphenyl)-1-methyl-6-trifluoromethyl-2(1H)-pyridone was dissolved in 5 ml of DMF, and dropwise added thereto, followed by stirring for 2 hours. The reaction mixture was poured into water and extracted with ethyl ether. The extract was dried over magnesium sulfate. Then, the solvent was distilled off under reduced pressure. Then, the obtained residue was purified by silica gel column chromatography to obtain 0.34 g (yield: 91%) of the desired product. Melting point: 99-101° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06472348B1 |
| Source dataset | uspto-grants-2002_10 |
| ORD ID | ord-98da191ab0da446f809cbbcc5ecc1c06 |
| Source note | uspto-grants-2002_10 |