Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 23440678 | HCID 23440678 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 22386479 | HCID 22386479 | — |
Reaction Steps
Under exclusion of air, 771 mg (2.9 mmol) 4-[3-(pyridin-3-yl)propyl]phthalazin-1(2H)-one in 14 ml acetonitrile is mixed with 1.11 g (7.25 mmol) phosphoryl chloride and 1.45 ml 4 N HCl in dioxane and stirred for 36 h at 45° C. Then 50 ml water is added, the reaction mixture adjusted to alkaline pH with sat. Na2CO3 solution and immediately extracted 3 times with EtOAc. Drying (Na2SO4) of the organic phases and evaporation yield the title compound; FAB-MS (M+H)+=284.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07329660B2 |
|---|
| Source dataset | uspto-grants-2008_02 |
|---|
| ORD ID | ord-70004534858b41799b23162299605117 |
|---|
| Source note | uspto-grants-2008_02 |
|---|
