Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acetic-formic anhydride | HCID 75269 | — |
| Reactant | HCID 18980999 | HCID 18980999 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 18980960 | HCID 18980960 | 78.3% |
Reaction Steps
To 3.0 g (6.7 mmole) of N-(4-trifluoromethylphenyl)-3-(4-propoxyphenyl)-4-(N-propylamino)-4,5,-dihydro-1H-pyrazole-1-carboxamide (Example 586) dissolved in 25 ml of ethyl acetate and cooled to 0° C., was added 2.4 g (30 mmole) of pyridine and 4.0 g (28 mmole) of formic acetic anhydride mixture (Example 621a). After 30 minutes, the reaction mixture was washed with water and brine, concentrated in vacuo, and chromatographed over silica gel using hexanes and ethyl acetate to yield 2.5 g of the desired compound, mp 161°-163° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05798311 |
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| Source dataset | uspto-grants-1998_08 |
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| ORD ID | ord-298edea4f19645388b55eff9618c32a9 |
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| Source note | uspto-grants-1998_08 |
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