Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 178490938 | HCID 178490938 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 178511625 | HCID 178511625 | 41.9% |
Reaction Steps
The solid from 62B was dissolved in TFA and heated to 70° C. for 1 h and then cooled to room temperature and purified by preparative HPLC (Phenomenex Axia Luna 5 micron 30×100 mm) to obtain the pure product 6-((trans-4-aminocyclohexyl)amino)-N-(2-fluoro-4-pyridinyl)-8-(2-pyridinylamino)imidazo[1,2-b]pyridazine-3-carboxamide (23 mg, 0.050 mmol, 41.9% yield) HPLC Rt=1.542 minutes (Phenomenex Luna 5 micron C18 4.6×30 mm: 0 to 100 B in 2 min with 1 min hold time, Flow rate=5 mL/min, detection at 254 nm, Solvent A: 10% methanol/90% water/0.1% TFA; Solvent B: 10% water/90% methanol/0.1% TFA). [M+H]=462.17.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08389527B2 |
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| Source dataset | uspto-grants-2013_03 |
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| ORD ID | ord-1367e5b114f94913b5cd9759f6c364fe |
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| Source note | uspto-grants-2013_03 |
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