HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21188137, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | HCID 9950049 | HCID 9950049 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 21188137 | HCID 21188137 | — |
Reaction Steps
To a solution of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-ethynylpyrazole (0.345 g) in acetonitrile (5 ml) was added p-toluenesulphonic acid (0.5 g) and the mixture was stirred at room temperature for 2 hours and then poured into water (100 ml) and ether (100 ml). The organic layer was separated, washed with saturated aqueous sodium hydrogen carbonate solution (50 ml), brine (50 ml), dried (Na2SO4) and evaporated. The residue was purified by column chromatography on silica gel (40 g) eluted with dichloromethane:hexane (10:1). Combination and evaporation of suitable fractions gave the title compound as a white crystalline solid, m.p. 200-1° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06028096 |
| Source dataset | uspto-grants-2000_02 |
| ORD ID | ord-6b2881c99ec54d5480ada08efeaaa44b |
| Source note | uspto-grants-2000_02 |