Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Chloro-3,5-difluoroaniline | HCID 2736494 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Solvent | Water | HCID 962 | — |
| Product | 3,5-Difluoroaniline | HCID 96595 | 92% |
Reaction Steps
Into a 500 ml SUS autoclave, 45.4 g (purity: 98%, 0.272 mol) of 2-chloro-3,5-difluoroaniline, 1.84 g of 5% palladium-carbon, 30.2 g (0.299 mol) of triethylamine and 45.4 g of water were introduced, and hydrogen gas was sealed in. Then, the mixture was reacted under a hydrogen gas pressure of 15 kg/cm2 at a temperature of 100° C. for 4 hours. Then, the reaction solution was cooled to 50° C. Then, palladium-carbon was filtered off, and 50 g of a 25% sodium hydroxide aqueous solution was added. The mixture was stirred and left to stand still. Then, the oil layer was separated. Then, this oil layer was distilled to recover 28.5 g of triethylamine, and then 32.3 g (purity: 99%, yield: 91.0%) of 3,5-difluoroaniline was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05399767 |
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| Source dataset | uspto-grants-1995_03 |
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| ORD ID | ord-46277cd71d3e4c0e8802999a46e200dd |
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| Source note | uspto-grants-1995_03 |
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