Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | HCID 13686005 | HCID 13686005 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 13686023 | HCID 13686023 | — |
Reaction Steps
To a 2.5 g amount of 4-[7-(3-pyridyl)[1,2,4]-triazolo[1,5-a]pyrimidin-2-yl]-1-piperazinecarboxylic acid benzyl ester was added 5.0 ml of hydrobromic acid (31% in glacial acetic acid). The mixture was allowed to react for 4 hours then was cooled to room temperature. Anhydrous ether was added, the mixture was swirled and the liquid decanted. This step was repeated several times. The residual precipitate was dissolved in water and the solution was filtered. The filtrate was made basic with 5N sodium hydroxide and extracted several times with dichloromethane. The extracts were combined and heated to boiling, then hexane was added to crystallize the product. Cooling and filtration gave 1.10 g of the deseired product as pale yellow crystals, mp 156°-158° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04582833 |
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| Source dataset | uspto-grants-1986_04 |
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| ORD ID | ord-93fc97a3037642108237da0c3777044c |
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| Source note | uspto-grants-1986_04 |
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