Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phthalazine | HCID 9207 | — |
| Reactant | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Reactant | 3-Bromo-4-ethylaniline | HCID 22345617 | — |
| Solvent | Ammonia | HCID 222 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 10114725 | HCID 10114725 | — |
Reaction Steps
Under N2-atmosphere, 0.73 g (3.7 mMol) 3-bromo-4-ethyl-aniline and 0.82 ml 4 N HCl/dioxane are added to 1.00 g (3.5 mMol) 1-chloro-4-[2-methoxy-pyridin-4-yl)methyl]phthalazine in 12 ml methanol, and the mixture is stirred for 2 h at 70° C. After cooling, the resulting yellow solution is diluted with EtOAc and 2.5% NH3 solution, and the aqueous phase is removed and extracted twice with EtOAct. The organic phases are washed with water and brine, dried (Na2SO4) and evaporated with a RE. After addition of DIPE to the residue, the title compound crystallizes out: M.p. 133-135° C.; FAB-MS: (M+H)+=449/451; HPLC(Grad20-100) tRet=11.4.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08034814B2 |
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| Source dataset | uspto-grants-2011_10 |
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| ORD ID | ord-da7711da6bec43b4af875cb40c355db2 |
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| Source note | uspto-grants-2011_10 |
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