Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-Chloroaniline | HCID 7812 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 19973081 | HCID 19973081 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 19973119 | HCID 19973119 | 24.3% |
Reaction Steps
A mixture of 100 mg of ethyl 3-(2,4-difluorophenyl)-2,2-difluoro-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)butyrate and 370 mg of 4-chloroaniline was subjected to reaction at 150°-160° C. for 5 hours. The reaction mixture was cooled to room temperature. Thereto were added 10 ml of ethyl acetate and 5 ml of water. The resulting solution was adjusted to pH 2.0 with 6N hydrochloric acid. The organic layer was separated, washed with a saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. Thereafter, the solvent was removed by distillation under reduced pressure. The residue obtained was purified by a column chromatography (eluant: toluene/ethyl acetate=1/1) to obtain 30 mg of N-(4-chlorophenyl)-3-(2,4-difluorophenyl)-2,2-difluoro-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)butanamide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05605921 |
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| Source dataset | uspto-grants-1997_02 |
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| ORD ID | ord-d0a3d69e5ec540ca8db7919d1a0e63e9 |
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| Source note | uspto-grants-1997_02 |
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