Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tributylamine | HCID 7622 | — |
| Reactant | Diethyl phenylmalonate | HCID 66514 | — |
| Reactant | HCID 178509138 | HCID 178509138 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178517358 | HCID 178517358 | 50% |
Reaction Steps
20 g (124.1 mmol) 5-Pyridine-2-yl-4H-[1,2,4]triazole-3-ylamine and 52.8 g (223.4 mmol) diethyl phenylmalonate are heated in 48.8 mL (204.8 mmol) tributylamine at 180° C. over night. After addition of additional 27 mL diethyl phenylmalonate the reaction mixture is heated for another night at 180° C. The reaction mixture is diluted with water and 2N NAOH and extracted three times with methyl-tert.butylether. The organic extracts are discarded after TLC check. The aqueous phase is acidified with 2M HCl until a pH of 1. The formed precipitate is collected by filtration, washed with plenty of water and dried. 18.96 g (45%) of the desired product are obtained which are used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08957064B2 |
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| Source dataset | uspto-grants-2015_02 |
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| ORD ID | ord-f9f2ee0c2d8446c889441ee3fc4e31ea |
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| Source note | uspto-grants-2015_02 |
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