Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanolamine | HCID 700 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 58046417 | HCID 58046417 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 58046394 | HCID 58046394 | — |
Reaction Steps
Ethanolamine (4.82 mL, 80 mmol) was added to a stirred mixture of 3-chloro-5-(4-fluorophenyl)pyridazine (2.08 g, 9.97 mmol) in Dioxane (40 mL) in a sealed tube. The mixture was heated to 120° C. overnight, treated with additional ethanolamine (1.2 mL, 20 mmol), and heated to 150° C. for 2 h. The mixture was cooled and poured into ethyl acetate (100 mL) and water (100 mL). The precipitate was filtered and dried to afford the title compound. 1H NMR (500 MHz, CD3SOCD3) δ 8.76 (d, 1H); 7.78 (dd, 2H); 7.36 (t, 2H); 7.02 (d, 1H); 6.85 (t, 1H); 4.78 (t, 1H); 3.58 (q, 2H); 3.45 (q, 2H). LRMS (APCI) calc'd for (C12H13FN3O) [M+H]+, 234.1. found 234.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08592425B2 |
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| Source dataset | uspto-grants-2013_11 |
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| ORD ID | ord-3122348ec4b240bb87cc0ad1e3db917e |
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| Source note | uspto-grants-2013_11 |
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