HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3,5-Bis(trifluoromethyl)benzylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 3,5-Bis-trifluoromethyl-benzaldehyde oxime | HCID 2726364 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 3,5-Bis(trifluoromethyl)benzylamine | HCID 521099 | 94.2% |
Reaction Steps
The second step of the process of the present invention was conducted as follows. At first, 5.03 g (19.6 mol) of 3,5-bis(trifluoromethyl)benzaldehyde oxime were dissolved in methanol followed by the addition of 3.0 g (82.3 mmol) of hydrogen chloride gas and 252 mg of a catalyst (i.e., activated carbon carrying thereon 5% palladium) and stirring for 5.5 hours in a hydrogen atmosphere at 10 atm and room temperature (approx. 25° C.). After removing the catalyst, ether was added to the reaction liquid, and the reaction liquid was neutralized with aqueous sodium hydroxide solution. As a result of analyzing the separated ether layer by gas chromatography, 3,5-bis(trifluoromethyl)benzylamine was formed at a yield of 94.2%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06331649B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-ad96e52346564eaab6af024ad26d6aef |
| Source note | uspto-grants-2001_12 |