Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethanolamine | HCID 8113 | — |
| Reactant | HCID 71533263 | HCID 71533263 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 71533325 | HCID 71533325 | — |
Reaction Steps
To a stirring solution of 3-amino-6-bromo-5-trifluoromethyl-pyrazine-2-carboxylic acid (2H-pyrazol-3-yl)-amide (Ex. 7)(50 mg, 0.142 mmol) in dry DMF (5 ml), diethanolamine (37.4 mg, 0.356 mmol) was added. The resulting solution was heated at 100° C. using microwave radiation for 66 hours. The reaction mixture was partitioned between EtOAc (20 ml) and water (20 ml), and the phases separated. The organic phase was washed with brine (10 ml), dried (MgSO4) and concentrated in vacuo to give an orange solid. Purification of the crude product by chromatography on silica eluting with iso-hexane/EtOAc (gradient of 0 to 50% EtOAc) yielded the title compound as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09056867B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-94d698fc57624c8dacbbec3de796c58b |
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| Source note | uspto-grants-2015_06 |
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