Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetate | HCID 175 | — |
| Reactant | p-Toluidine | HCID 7813 | — |
| Reactant | 1-Chloro-4-(4-pyridinylmethyl)phthalazine | HCID 1944609 | — |
| Solvent | Potassium Carbonate | HCID 11430 | — |
| Product | HCID 9818750 | HCID 9818750 | — |
Reaction Steps
A mixture of 0.384 g (1.5 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.482 g (4.5 mmol) p-toluidine is stirred for 1.5 h at 90° C. under a nitrogen atmosphere. The reaction mixture is then distributed between 30 ml acetate and 20 ml of 20% aqueous potassium carbonate solution. The organic phase washed with water and dried over anhydrous sodium sulfate is evaporated and the residue purified on silica gel by flash chromatography using acetate/methanol mixtures (50:1 to 9:1). Title compound is obtained after crystallization of the product-containing fractions from acetonitrile and drying under HV; m.p. 152-153° C.; ESI-MS: (M+H)+=327.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06710047B2 |
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| Source dataset | uspto-grants-2004_03 |
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| ORD ID | ord-0ee547c4878842c0b4af4db53c2fdb6f |
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| Source note | uspto-grants-2004_03 |
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