HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,5-Bis(trifluoromethyl)benzoic acid → N-(6-Chloro-4-phenyl-pyridazin-3-yl)-N-methyl-3,5-bis-trifluoromethyl-benzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,5-Bis(trifluoromethyl)benzoic acid | HCID 12889 | — |
| Reactant | 6-chloro-N-methyl-4-phenylpyridazin-3-amine | HCID 86698478 | — |
| Solvent | Ethylacetate heptane | HCID 21899848 | — |
| Product | N-(6-Chloro-4-phenyl-pyridazin-3-yl)-N-methyl-3,5-bis-trifluoromethyl-benzamide | HCID 71766226 | — |
Reaction Steps
The title compound was prepared in analogy to example 1, from (6-chloro-4-phenyl-pyridazin-3-yl)-methyl-amine (example 5, intermediate a) and 3,5-bis(trifluoromethyl)benzoic acid (CAS RN 725-89-3) and using a gradient of n-heptane:ethyl acetate (100:0 to 30:70) for the chromatographic purification. Another purification step using preparative HPLC (Gemini NX column) with a gradient of methanol:water with 0.05% formic acid (80:20 to 98:2) yielded the compound as a colorless solid (5%). MS (ESI+): m/z=460.064 ([M+H]+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08748434B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-afe5ec69d94b47b4b52ce27853dcb7b8 |
| Source note | uspto-grants-2014_06 |