HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 19609782, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 15869764 | HCID 15869764 | — |
| Reactant | Potassium methoxide | HCID 23664618 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 19609782 | HCID 19609782 | 75% |
Reaction Steps
A 25% solution of potassium methylate in dry methanol (4.4 ml, 15 mmol) is added to a solution of 3,5-difluoro-2,4,6-tris (1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine (9.1 g, 15 mmol; see (a) above) in dry methanol (50 ml). After 30 min at ambient temperature the reaction is stopped by adding 2 ml of water. The solvent is removed under reduced pressure and pentane/ethyl acetate (1/1 by volume) is added to the residue. After filtration through a bed of silica gel the filtrate is washed with a 2 N sodium hydroxide solution. After drying and filtration of the organic layer, the solvents are removed and the residue is washed with diisopropyl ether. One obtains colorless crystals (5.3 g 75% yield), m.p. 83° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05981437 |
| Source dataset | uspto-grants-1999_11 |
| ORD ID | ord-48d0734e8b1f4fd097bd02b9f6ef8fdb |
| Source note | uspto-grants-1999_11 |