Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Isopropanol | HCID 3776 | — |
| Reactant | HCID 19707182 | HCID 19707182 | — |
| Reactant | HCID 54558834 | HCID 54558834 | — |
| Solvent | Tetrahydrothiophene | HCID 1127 | — |
| Product | HCID 19707185 | HCID 19707185 | 53.3% |
Reaction Steps
A mixture of ethyl 4-(5-amino-2-pyridinyl)-1-piperazinecarboxylate (0.18 mol) and ethyl 2-[(dimethylamino)methylene]hydrazinecarboxylate (0.54 mol) in tetrahydrothiophene, 1,1-dioxide (50 ml) was stirred at 150° C. for 3 hours. The mixture was cooled till 100° C., 2-propanol was added until crystallization. The precipitate was filtered and recrystallized from methanol; yielding 30.5 g ethyl 4-[5-(2,3-dihydro-3-oxo-4H-1,2,4-triazol-4-yl)-2-pyridinyl]-1-piperazinecarboxylate (53.3%); mp. 220.8° C. (interm. 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05710156 |
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| Source dataset | uspto-grants-1998_01 |
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| ORD ID | ord-edf7113356cb452ab444adee9017ad15 |
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| Source note | uspto-grants-1998_01 |
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