Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 22386451 | HCID 22386451 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 22386466 | HCID 22386466 | — |
Reaction Steps
Under N2-atmosphere, 217 mg (0.818 mmol) 4-[2-(6-methylpyridin-3-yl)ethyl]phthalazin-1(2H)-one in 3.3 ml acetonitrile is mixed with 187 μl (2.04 mmol) phosphoryl chloride and 0.41 ml 4 N HCl in dioxane and stirred for 9 h at 60° C. After cooling to RT, 2.6 ml H2O, followed by a solution of 0.5 ml sat. NH3 and 5 ml H2O is added. Immediate extraction with 3 portions of EtOAc, washing of the organic layers with water and brine, drying (Na2SO4) and evaporation yield the title compound; FAB-MS (M+H)+=284.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07329660B2 |
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| Source dataset | uspto-grants-2008_02 |
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| ORD ID | ord-ab33100413704a44b6dad3b505eddb15 |
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| Source note | uspto-grants-2008_02 |
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