Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 71666317 | HCID 71666317 | — |
| Solvent | Ethylene Glycol | HCID 174 | — |
| Product | HCID 89717988 | HCID 89717988 | — |
Reaction Steps
To a suspension of 2-{4-[5-(1-ethyl-1H-pyrazol-4-ylamino)-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl]-phenyl}-propan-2-ol (138 mg, 0.38 mmol) in ethane-1,2-diol (1 ml) is added toluene-4-sulfonic acid monohydrate (89 mg, 0.42 mmol). The reaction mixture is stirred for 16 hours at ambient temperature. The mixture is then heated to 80° C. and the resulting clear solution is stirred at this temperature for 1 hours. The reaction mixture is cooled to room temperature and water is added. The resulting precipitate is filtered off and washed with water. The residue is chromatographed on a silica gel column with dichloromethane/methanol as eluent to afford 2-(1-{4-[5-(1-ethyl-1H-pyrazol-4-ylamino)-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl]-phenyl}-1-methyl-ethoxy)-ethanol (“A127”) as yellow powder; HPLC/MS1.67 min (A), [M+H] 409;
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09409914B2 |
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| Source dataset | uspto-grants-2016_08 |
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| ORD ID | ord-820186b1cea44d4eb79c39b1490afacc |
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| Source note | uspto-grants-2016_08 |
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