Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 67318545 | HCID 67318545 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 59427323 | HCID 59427323 | — |
Reaction Steps
4-(4-Chlorophenyl)-N-(4-(6,7-dimethoxy-1,5-naphthyridin-4-ylthio)phenyl)phthalazin-1-amine (40 mg, 72 μmol) was added to a pyrex reaction tube along with 2 mL of 1:1 HBr:AcOH. The tube was sealed and the mixture was heated at 85° C. for 1.5 h. Upon cooling the mixture was diluted with water and brought to basic pH by dropwise addition of 6N NaOH. The solids were filtered, washed with water, and dried. The crude material was purified by silica gel chromatography, 10-50% 90/10/1 DCM/MeOH/NH4OH in DCM to provide 8-(4-(4-(4-chlorophenyl)phthalazin-1-ylamino)phenylthio)-3-methoxy-1,5-naphthyridin-2(1H)-one as a light yellow solid. MS: [M+H]=539.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07981891B2 |
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| Source dataset | uspto-grants-2011_07 |
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| ORD ID | ord-4de6bfaa4abf40e9a4ec8b551a7001c2 |
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| Source note | uspto-grants-2011_07 |
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