HuagongsheHuagongshe Chemistry Print Report · For research reference only
18-Crown-6 → HCID 18689507, compound
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 the mixture was stirred for 5 hours at 150°-155° C. After cooling, the reaction mixture was stirred with methyl tert-butyl ether and separated from the inorganic precipitate. The filtrate was extracted four times using water, dried and concentrated. The residue together with methylene chloride was filtered with suction through a silica gel frit and concentrated, giving 31.4 g (71% of theory) of the title compound of ηD24 1.4732 (Table III, No. 3.036).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05750705 |
| Source dataset | uspto-grants-1998_05 |
| ORD ID | ord-4a9382449c774a9cabecd70fc2edd7e8 |
| Source note | uspto-grants-1998_05 |