Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 67317949 | HCID 67317949 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 12231775 | HCID 12231775 | — |
Reaction Steps
In a 150 mL sealed tube, dissolved N-(2,4-dimethoxybenzyl)-4-phenylphthalazin-1-amine (3.00 g, 8.1 mmol) in acetic acid (40 mL). Hydrobromic acid (48% aqueous) (2.6 mL, 24 mmol) was added and the tube was stirred at 90° C. for 3 h. The solution was cooled to RT, and slowly poured into water, which caused a pink solid to crash out. The solid was filtered and rinsed with water. The product containing filtrate was slowly poured into saturated sodium carbonate. The aqueous phase was extracted with DCM, washed twice with water, dried with Na2SO4, filtered through flitted funnel, and concentrated to yield 4-phenylphthalazin-1-amine as light yellow solid. MS [M+H]=222; Calc'd 221.3 for C14H11N3.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08557816B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-d789706e46ba4e26931e21c8adea8997 |
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| Source note | uspto-grants-2013_10 |
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