HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 20131579, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | HCID 13021647 | HCID 13021647 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 20131579 | HCID 20131579 | 65.1% |
Reaction Steps
20.0 g of 1-fluoro-1-(1H-1,2,4-triazol-1-yl)-3,3-dimethyl-2-butanone are added dropwise to a solution of 13.5 g of potassium tertiary butylate in 100 ml of tetrahydrofuran. After the mixture has been stirred for 0.5 hour, 15.6 g of methyl iodide are added dropwise and the mixture is stirred for 18 hours at 60° C. After cooling, the reaction mixture is taken up in ice water and extracted with ethyl acetate. The combined organic phases are washed with water and saturated sodium chloride solution, dried over sodium sulfate and evaporated. Distillation of the oily residue gives 14.0 g of 2-fluoro-2-(1H-1,2,4-triazol-1-yl)-4,4-dimethyl-3-pentanone, boiling point 48°-50° C./0.013 mbar.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04758670 |
| Source dataset | uspto-grants-1988_07 |
| ORD ID | ord-161e274492244bc58981affa7d0d5c44 |
| Source note | uspto-grants-1988_07 |