Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Chloro-1-[(3,5-dichloropyridin-4-yl)methyl]-6-methoxyphthalazine | HCID 18629210 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18381680 | HCID 18381680 | 50% |
Reaction Steps
A solution of imidazole (0.814 g, 11.21 mmoles) in dry DMF (30 ml) was stirred under N2 at room temperature and added with NaH (8.46 mmoles). After 30 minutes 4-chloro-1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine (2 g, 5.64 mmoles), prepared as described in example 45, in dry DMF (30 ml) was added. The mixture was heated at 80° C. for 3.5 hours, cooled, poured into water/ice and extracted three times with CH2Cl2. The organic phase was washed with water, anhydrified and concentrated to give a solid which was flash chromatographed (eluent: ethyl acetate) yielding 0.9 g of the title compound (yield: 50%). m.p. 250° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06492360B1 |
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| Source dataset | uspto-grants-2002_12 |
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| ORD ID | ord-496690b7505f4cadbdb496e7ee75c3c4 |
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| Source note | uspto-grants-2002_12 |
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