Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 57929844 | HCID 57929844 | — |
| Product | HCID 57929870 | HCID 57929870 | 58% |
Reaction Steps
Ethyl 2-cyano-2-(3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)acetate (1.16 g, 4.24 mmol) was suspended in 5N HCl (15 mL, 75 mmol) then heated at about 105° C. for about 20 min. The mixture was cooled to ambient temperature then concentrated under reduced pressure. The residue was partitioned between saturated aqueous NaHCO3 (25 mL) and EtOAc (50 mL). The aqueous layer was extracted with EtOAc (25 mL), the combined organics were dried over MgSO4, filtered and concentrated under reduced pressure. The oil was purified by flash chromatography on silica gel using DCM/MeOH (95:5) as an eluent to give the title compound (0.493 g, 58%): LC/MS (Table 1, Method g) Rt=1.41 min; MS m/z: 202.1 (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-bef7b06a888d414881d702b375d9b40d |
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| Source note | uspto-grants-2012_05 |
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