Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | HCID 12017517 | HCID 12017517 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 12017518 | HCID 12017518 | — |
Reaction Steps
A 3.0 ml portion of ethylenediamine was added to a mixture of 1.0 g of 2-(benzotriazol-1-yloxy)-4-(4-methylanilino)pyrimidine-5-carboxamide and 30 ml of acetonitrile, followed by stirring at room temperature for 1 hour and 40 minutes. Water was added to the reaction mixture, followed by extraction with a chloroform-isopropanol mixed solution. The resulting organic layer was dried over anhydrous sodium sulfate and concentrated under a reduced pressure and then the thus obtained residue was purified by silica gel column chromatography (eluting solvent; chloroform:methanol:aqueous ammonia) . By recrystallizing the thus obtained colorless solid from an ethyl acetate-ethanol mixed solvent, 471 mg of 2-(2-aminoethylamino)-4-(4-methylanilino)pyrimidine-5-carboxamide was obtained (colorless crystals).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06432963B1 |
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| Source dataset | uspto-grants-2002_08 |
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| ORD ID | ord-f50b98aa2401497a86ef34b61f7abe0d |
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| Source note | uspto-grants-2002_08 |
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