Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 86594451 | HCID 86594451 | — |
| Reactant | 2,6-diamino-5-nitropyrimidin-4(3H)-one | HCID 135461662 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 136341860 | HCID 136341860 | — |
Reaction Steps
A 3-necked 500 mL round bottomed flask equipped with stirrer, temperature probe and reflux condenser was charged with the amine 69 (1.49 g, 5 mmol), 2,4-diamino-5-nitropyrimidin-6-one (1.56 g, 5.35 mmol) and n-butanol (20 mL). The resultant thin slurry was subjected to heating at 40–45° C. over 15 minutes. Triethylamine (0.71 mL, 5.1 mmol) was added slowly over a period of 2 minutes. The reaction mixture was stirred at about 70° C. for 1 h. HPLC data showed that the reaction was almost complete. At this point, five washes of 25 mL of water was given to the reaction mixture at 70° C. The last wash was almost colorless. The crude product, 70, in n-butanol was used without further purification in the next reaction.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07034152B2 |
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| Source dataset | uspto-grants-2006_04 |
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| ORD ID | ord-8c6a934906d143b991c7b62a1b0e5990 |
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| Source note | uspto-grants-2006_04 |
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