HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylphosphine → HCID 89768806, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Reactant | (1-Methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)methanol | HCID 58456726 | — |
| Reactant | HCID 131734536 | HCID 131734536 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 89768806 | HCID 89768806 | 90.9% |
Reaction Steps
To a mixture of tri-n-butylphosphine (0.415 mL), methyl(4-chloro-6-hydroxy-2-methyl-1-benzothiophen-3-yl)acetate (150 mg) and (1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)methanol (105 mg) in THF (4.0 mL) was added ADDP (419 mg) at room temperature. The mixture was stirred at room temperature under nitrogen atmosphere for 1 h. The mixture was concentrated. To the residue was added IPE and the precipitate was filtered off and the filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (NH, EtOAc/hexane) and silica gel column chromatography (EtOAc/hexane) to give the title compound (218 mg) as a colorless solid. The solid was crystallized from EtOAc-hexane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09238639B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-eedfa38b1bed4868b8ad2d1d3972132a |
| Source note | uspto-grants-2016_01 |