Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 70980124 | HCID 70980124 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 66571316 | HCID 66571316 | 88% |
Reaction Steps
To a solution of 2-(5-chloro-2-methyl-phenyl)-5-(2-methylamino-pyrimidin-4-yl)-1H-pyrrole-3-carbonitrile (1.15 g, 3.55 mmol) in TFA (15.0 mL) were sequentially added water (2.25 mL) and 98% sulfuric acid (4.5 mL) under efficient stirring. The mixture was allowed to stir for 8 h at 70° C. and then was diluted by drop wise addition of water (45 mL). The reaction mixture was made basic (pH 10-12) by adding 30% aqueous ammonia (15 mL) under stirring. The precipitated solid was collected by filtration, washed with water and finally dried in a vacuum oven at 50° C. affording the title compound as an off-white solid (1.07 g, 88%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08912200B2 |
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| Source dataset | uspto-grants-2014_12 |
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| ORD ID | ord-0cf6313d5b444429b4a965bad9e2b366 |
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| Source note | uspto-grants-2014_12 |
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