HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylphosphine → HCID 57652739, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | HCID 66704182 | HCID 66704182 | — |
| Reactant | HCID 136342877 | HCID 136342877 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 57652739 | HCID 57652739 | 30% |
Reaction Steps
Nitrogen is bubbled through a solution of [5-cyclopropyl-3-(2,6-dichloro-phenyl)-3H-[1,2,3]triazol-4-yl]-methanol (0.23 g, 0.80 mmol) and 6-(4-hydroxy-2-methyl-phenyl)-1-isopropyl-1H-indazole-3-carboxylic acid methyl ester (0.2 g, 0.62 mmol) in toluene (10 mL) for 10 minutes. Tri-n-butyl phosphine (0.21 mL, 1.05 mmol) is added. Nitrogen is bubbled for an additional 10 min followed by addition of 1,1′-(azocarbonyl)-dipiperidine (0.27 g, 1.05 mmol). The reaction is stirred at room temperature for 18 h. The crude reaction is concentrated onto silica and chromatographed (40 g SiO2, 0% to 40% EtOAc/Hexanes) to yield the title compound (0.11 g, 30%). LC-ES/MS m/e 590.0 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08106077B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-d34d72beec974030b63c88c222a6e85b |
| Source note | uspto-grants-2012_01 |