Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 18-Crown-6 | HCID 28557 | — |
| Reactant | Sulfolane | HCID 31347 | — |
| Reactant | Potassium Fluoride | HCID 522689 | — |
| Reactant | HCID 18689506 | HCID 18689506 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | HCID 18689507 | HCID 18689507 | — |
Reaction Steps
47.3 g (0.175 mol) of 2,5-dichloro-6-propargyloxy-3-trifluoromethylpyridine, 0.5 g (1.89 mmol) of 18-crown-6 and 15.2 g (0.263 mol) of potassium fluoride were added to 150 ml of sulfolane and it was stirred at 150-155° C. for 5 hours. After cooling, the reaction mixture was stirred with methyl tert-butyl ether and separated off from the inorganic precipitate. The filtrate was extracted four times with water, dried and concentrated. The residue was filtered with suction with methylene chloride through a suction filter containing silica gel and concentrated, 31.4 g (71% of theory) of the title compound of n24D =1.4732 being obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06107253 |
|---|
| Source dataset | uspto-grants-2000_08 |
|---|
| ORD ID | ord-6583b03e5599430b8c5decb62ad679dd |
|---|
| Source note | uspto-grants-2000_08 |
|---|