Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | HCID 57929849 | HCID 57929849 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 57929959 | HCID 57929959 | 43% |
Reaction Steps
The 2-(3-(2,4-difluorophenyl)-4-(3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)-1H-pyrazol-1-yl)ethyl methanesulfonate (0.24 g, 0.52 mmol; Preparation #W.1) was dissolved in MeOH (4 mL) then morpholine (0.36 g, 4.2 mmol) was added. The mixture was heated at about 70° C. in an oil bath for about 2 h then cooled and concentrated under reduced pressure. The crude material was purified by RP-HPLC (Table 1, Method d). The appropriate fractions were concentrated under reduced pressure then basified with 2 N NaOH. Extraction of the solution with EtOAc followed by drying of the organic extract over MgSO4 and then filtration prior to concentrating under reduced pressure gave the title compound (0.10 g, 43%): LC/MS (Table 1, Method a) Rt=2.09 min; MS m/z: 454.2 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08188083B2 |
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| Source dataset | uspto-grants-2012_05 |
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| ORD ID | ord-848b6908dfc442ec91c2b53f4239de51 |
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| Source note | uspto-grants-2012_05 |
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