Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22013570 | HCID 22013570 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 21712165 | HCID 21712165 | 93% |
Reaction Steps
6.75 g of 3-(3-fluoro-5-chloro-2-pyridyl)-4-methyl-5methoxycarbonyl-1-methyl-[1H]-pyrazole are suspended in 40 ml of dimethyl sulfoxide. 14.3 ml of a 2 molar sodium hydroxide solution are added dropwise, while cooling occasionally in an ice-bath (temperature <30° C.). The thick yellow-brown suspension is stirred at 22° C. for 2 hours. The resulting suspension is then introduced into ice-water and the pH is brought to 1 with 2 molar hydrochloric acid. The slurry formed is filtered with suction and the solid is washed thoroughly with cold water and then dried in vacuo at 60° C. 5.97 g of the desired title compound are obtained as a beige solid of melting point 194-196° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06204221B1 |
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| Source dataset | uspto-grants-2001_03 |
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| ORD ID | ord-5e6a9c2c4b044c22a5d037137afd1157 |
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| Source note | uspto-grants-2001_03 |
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