HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 178526652, compound → HCID 178507665, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 178526652 | HCID 178526652 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178507665 | HCID 178507665 | 97.1% |
Reaction Steps
A mixture of 4-(trans-4-hydroxycyclohexylamino)-3-nitrobenzotrifluoride (4.0 g) and 10% palladium on activated carbon (400 mg) in a mixture of methanol (20 mL) and dioxane(20 mL) was stirred under hydrogen atmosphere (3 atm) at ambient temperature for 4 hours. The reaction mixture was filtered through a celite pad, and the filtrate was concentrated in vacuo. The residue was subjected to a silica gel column chromatography eluting with a mixture of chloroform and methanol (20:1). The obtained substance was triturated with petroleum ether to give 3-amino-4-(trans-4-hydroxycyclohexylamino)benzotrifluoride (3.5 g) as a pale orange solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06582351B1 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-66c3eb82e2b449eca19504b0ede5eac6 |
| Source note | uspto-grants-2003_06 |