Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Fluoro-2-(trifluoromethyl)benzoyl chloride | HCID 605680 | — |
| Reactant | HCID 66971335 | HCID 66971335 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66971277 | HCID 66971277 | 59% |
Reaction Steps
Charge a 4 mL reaction vial with 4-(4-(4-(methylamino)piperidine -1-yl)phthalazin -1-yl)benzonitrile dihydrochloride (44.7 mg, 0.107 mmol), dichloromethane (1 mL), and triethylamine (0.0598 mL, 0.429 mmol). Flush the reaction vial with nitrogen and add 4-fluoro-2-(trifluoromethyl)benzoyl chloride (033 g. 0.14 mmol). Cap the vial and allow the reaction to stir at room temperature overnight. Evaporate to a residue and purify using silica gel chromatography (40:60, ethyl acetate:hexane, then ethyl acetate). Add 1 N HCl in diethyl ether to a solution of the isolated product in dichloromethane/methanol and remove the solvents by placing under a stream of nitrogen gas. Dry in a vacuum oven at 50° C. to obtain the title compound (36.0 mg. 59%). ES/MS m/z 533.8 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07981892B2 |
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| Source dataset | uspto-grants-2011_07 |
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| ORD ID | ord-3269dd7e3a734705b1afdefcb2e50a8f |
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| Source note | uspto-grants-2011_07 |
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