HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylamine → HCID 178516959, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylamine | HCID 7622 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Diethyl phenylmalonate | HCID 66514 | — |
| Reactant | 6-bromo-1H-indazol-3-amine | HCID 2786631 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178516959 | HCID 178516959 | 97.4% |
Reaction Steps
9.9 g (46.7 mmol) 6-Bromo-1H-indazol-3-ylamine, 11 g (46.7 mmol) diethyl phenylmalonate and 19.8 mL (83.1 mmol) tributyl amine were heated for 15 h at 180° C. The reaction mixture was treated with 2M sodium hydroxide and water and extracted three times with tert-butyl methyl ether. The organic phase was discarded and the aqueous phase was acidified with conc. hydrochloric acid. The precipitate was collected by filtration and washed with water to obtain the desired product (16.2 g) which was however contaminated and which was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08987286B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-e2ccdc84123245c1bc45a47123014ca7 |
| Source note | uspto-grants-2015_03 |