Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Acetone | HCID 180 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 3-(Methylthio)-1,2,4-triazol-5-amine | HCID 78471 | — |
| Reactant | Ethyl 1-benzyl-3-oxopiperidine-4-carboxylate hydrochloride | HCID 2723880 | — |
| Product | HCID 178503363 | HCID 178503363 | 91% |
Reaction Steps
A mixture of 39.05 g (0.3 mole) of 5-amino-3-methylthio-1H-1,2,4-triazole, 1-benzyl-4-carbethoxy-3-oxo-piperidine-hydrochloride and 110 ml of acetic acid is heated to boiling for 6.5 hours. The reaction mixture is allowed to stand overnight, the precipitate is filtered and washed with acetone. Thus 115.30 g of the crude product are obtained. The crude product is dissolved in 130 ml of hot pyridine, and to the pyridine solution 400 ml of acetone are added. The precipitated crystals are filtered, washed with acetone, the product is dissolved in 270 ml of pyridine and 1000 ml of acetone are added to the pyridine solution. The precipitated crystals are filtered and washed with acetone. Thus 89.3 g of the desired compound are obtained, yield 91%, m.p.: 232°-234° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04831029 |
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| Source dataset | uspto-grants-1989_05 |
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| ORD ID | ord-3d7198b5a9e74a9da613b9aa5ed9ba07 |
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| Source note | uspto-grants-1989_05 |
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