Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 58335579 | HCID 58335579 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178515976 | HCID 178515976 | — |
Reaction Steps
In step 16-1, a suspension of (R)-6-(2-(3-fluorophenyl)pyrrolidin-1-yl)-3-(6-fluoropyridin-2-yl)imidazo[1,2-b]pyridazine (16 g, 42 mmol) in acetic acid (150 mL) was heated overnight at 120° C. (approx. 20 hours). The suspension turned clear after heating. The mixture was concentrated under vacuum to give a brown oil. The oil was dissolved in CH2Cl2 (750 mL) and washed with saturated NaHCO3 (300 mL×3), brine (300 mL×2). The organic layer was separated, dried over (Na2SO4) and concentrated to give 15.5 g of the crude (R)-6-(6-(2-(3-fluorophenyl)pyrrolidin-1-yl)imidazo[1,2-b]pyridazin-3-yl)pyridin-2-ol (16-1) which was used in the next step without further purification. LC/MS: 376.2 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08507488B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-88cedbbbfdb24c00a929800cd6512835 |
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| Source note | uspto-grants-2013_08 |
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