HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 68799100, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 86616967 | HCID 86616967 | — |
| Reactant | HCID 178418416 | HCID 178418416 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 68799100 | HCID 68799100 | 73% |
Reaction Steps
To a solution of 10.20 g (0.029 mol) 5-bromo-3-(4-trifluoromethoxy-phenyl)-pyrazin-2-ylamine in 100 ml methanol and 40 ml ethyl acetate was added 0.500 g (0.0006 mol) PdCl2 dppf CH2Cl2 ([1,1′-Bis(diphenylphosphino)ferrocene]palladium(II) chloride dichloromethane adduct, Cas Registry No. [95464-05-4]) and 8.113 ml (5.9 g, 0.058 mol) triethylamine and the mixture was stirred at 110° C. under 70 bar carbon monoxide pressure for 4 h. The solvents were evaporated and the residue was purified by chromatography on silica gel with a gradient of 100% heptane to 100% ethyl acetate to yield 6.800 g (73% yield) of the title compound as off white crystalline solid. MS (ISP) (M+H+)=314.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07629346B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-b706abd63fa846debb30998eb89cb580 |
| Source note | uspto-grants-2009_12 |