Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Phosphoric Acid | HCID 1004 | — |
| Reactant | 2,6-Diaminopyridine | HCID 8861 | — |
| Reactant | Ethyl 4-chloroacetoacetate | HCID 69484 | — |
| Product | HCID 178507291 | HCID 178507291 | 54.4% |
Reaction Steps
32.9 g (0.2 mol) of ethyl 4-chloroacetoacetate is dripped into a suspension of 21.8 g (0.2 mol) of 2,6-diaminopyridine in 100 ml of 85% strength phosphoric acid. The reaction mixture is stirred for 3 hours at 90° C., cooled and poured into ice water, followed by neutralization with concentrated aqueous ammonia solution. The precipitate is suction filtered, stirred into water again and finally boiled with acetonitrile. 22.8 g (54%) of the title compound is obtained; m.p.: >280° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05258356 |
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| Source dataset | uspto-grants-1993_11 |
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| ORD ID | ord-8272b810451d40608f12ec452d698c7b |
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| Source note | uspto-grants-1993_11 |
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