HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67070043, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethanamine, 2,2,2-trifluoro- | HCID 9773 | — |
| Reactant | HCID 86638345 | HCID 86638345 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 67070043 | HCID 67070043 | 37% |
Reaction Steps
step 2—A solution of 312 (0.059 g, 0.1 mmol) and 2,2,2-trifluoroethylamine (0.5 mL) in NMP (1.0 mL) in a screw-capped test tube was heated to 100° C. After 18 h the solution was cooled to RT poured into H2O and extracted with EtOAc. The combined organics were washed sequentially with H2O and brine, dried (Na2SO4), filtered and concentrated in vacuo. The crude product was purified by SiO2 chromatography eluting with an EtOAc/hexane (6% to 60% EtOAc) to afford 0.029 g (37%) 6-(2,2,2-trifluoro-ethylamino)-pyridazine-3-carboxylic acid [5-(2-benzyloxy-pyridin-3-yl)-3-tert-butyl-2-methoxy-phenyl]-amide (314) as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08273773B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-3af448e54f374523ba142ba018e3f65a |
| Source note | uspto-grants-2012_09 |