Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 67309598 | HCID 67309598 | — |
| Reactant | HCID 68856325 | HCID 68856325 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57677077 | HCID 57677077 | 6.5% |
Reaction Steps
To a solution of 4-{2-[(5-chlorothieno[2,3-d]pyrimidin-4-yl)amino]ethyl}phenol (0.152 g, 0.5 mmol) and 5-(tert-butyl)-3-(6-fluoropyridin-2-yl)-3H-[1,3,4]oxadiazol-2-one (0.119 g, 0.5 mmol) in anhydrous DMF (4 mL) was added 60 percent sodium hydride in mineral oil (30 mg, 0.75 mmol) portionwise. The mixture was then stirred at 100° C. overnight. After cooling the reaction was quenched with methanol. The solvent was removed in vacuo and the residue was triturated in CH2Cl2 and water. The organic phase was separated, dried over anhydrous Na2SO4, filtered, concentrated, and purified on preparative HPLC to give the decarboxylated product as a brownish foam, 16 mg, 0.03 mmol, 6.5 percent yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07531482B2 |
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| Source dataset | uspto-grants-2009_05 |
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| ORD ID | ord-360676f7054c4803b2b5b0b227ab094f |
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| Source note | uspto-grants-2009_05 |
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