HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylamine → HCID 178432407, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylamine | HCID 7622 | — |
| Reactant | 3-Amino-5-methyl-4H-1,2,4-triazole | HCID 234610 | — |
| Reactant | Diethyl (3-fluorophenyl)propanedioate | HCID 12965551 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 178432407 | HCID 178432407 | 88.7% |
Reaction Steps
5 g (51.87 mmol) 3-Amino-5-methyl-1,2,4-triazole, 16.2 g (67.4 mmol) diethyl (3-fluorophenyl)malonate and 20.4 mL tributylamine are stirred at 180° C. over night. The mixture is diluted with 2N NaOH solution and water and extracted three times with methyl-tert. butylether. These organic extracts are discarded. The aqueous phase is acidified at 0° C. with concentrated HCl until pH 3. The white precipitate is collected by filtration, washed with water (4 L) and dried in vacuo at 50° C. 11.97 g (88.7%) of the product are obtained and are used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957064B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-8f3ebf9e612a4a28a28a58bfe9f5fdfa |
| Source note | uspto-grants-2015_02 |