Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Maleic Acid | HCID 444266 | — |
| Reactant | HCID 178441801 | HCID 178441801 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 178441805 | HCID 178441805 | 89% |
Reaction Steps
5-Butyl-3-(6-(pyrrolidin-1-yl)hexyl)-1H-pyrazolo[4,3-d]pyrimidin-7-amine (197.3 mg) was treated with maleic acid (133 mg, 2.0 eq) before being slurried in IPA (2.0 mL). The resulting reaction mixture was heated to 70° C. resulting in a homogeneous solution which on aging at 70° C. started to precipitate solid. The resulting slurry was found to set solid at 70° C. therefore an additional IPA (2.0 mL) was added to mobilise the slurry. The resulting reaction mixture was allowed to cool slowly to 20° C. and was aged overnight at 20° C. before being filtered and washed with fresh IPA (2×4 mL) to yield a white solid which was oven dried at 40° C. in vacuo (90 mbar) overnight to afford the title compound (294 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09173872B2 |
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| Source dataset | uspto-grants-2015_11 |
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| ORD ID | ord-507e2396793c4ef5b1799f2fad80950c |
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| Source note | uspto-grants-2015_11 |
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