Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 67017177 | HCID 67017177 | — |
| Product | HCID 59427295 | HCID 59427295 | — |
Reaction Steps
A RBF was charged with 6-(3-chlorophenyl)-4-ethylpyridazin-3(2H)-one (1.50 g, 6.4 mmol) and phosphorus oxychloride (6.0 ml, 64 mmol). Hunig's base (1.2 ml, 7.0 mmol) was added to the mixture dropwise (slightly exothermic). The flask was fitted with a reflux condenser and a nitrogen inlet and the mixture was heated at 110° C. for 3 h. Upon cooling the reaction mixture was poured onto ice. 6N NaOH was added dropwise until pH 9 while keeping the mixture cold by gradual addition of ice. The solids were filtered, washed with water and dried to provide 3-chloro-6-(3-chlorophenyl)-4-ethylpyridazine as a peach colored solid. MS m/z=253 [M]+. Calc'd for C12H10Cl2N2: 253.13.
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-ea51b42e36314060965787a60dfedd38 |
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| Source note | uspto-grants-2013_10 |
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