Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetate | HCID 175 | — |
| Reactant | 4-Fluoroaniline | HCID 9731 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Chloro-4-(4-pyridinylmethyl)phthalazine | HCID 1944609 | — |
| Product | HCID 9949395 | HCID 9949395 | — |
Reaction Steps
A mixture of 0.511 g (2 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.576 ml (6 mmol) 4-fluoroaniline is heated for 2 h at 90° C. The residue is then distributed between acetate and 20% aqueous potassium carbonate solution. The organic phase washed with water and dried over sodium sulfate is evaporated and the residue purified on silica gel by flash chromatography using acetate/methanol mixtures (50:1 and 25:1). Title compound is obtained after crystallization of the product-containing fractions from acetonitrile and drying under HV (6 h, 100° C.); m.p. 129-131° C.; ESI-MS: (M+H)+=331.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06710047B2 |
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| Source dataset | uspto-grants-2004_03 |
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| ORD ID | ord-ac39a0f1f7a347668c01e5f18e9de5ef |
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| Source note | uspto-grants-2004_03 |
|---|