HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylphosphine → HCID 118667068, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Reactant | (2-Methyl-6-(trifluoromethyl)pyridin-3-yl)methanol | HCID 2760122 | — |
| Reactant | HCID 131734536 | HCID 131734536 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 118667068 | HCID 118667068 | 66.6% |
Reaction Steps
To a mixture of tri-n-butylphosphine (0.418 mL), methyl(4-chloro-6-hydroxy-2-methyl-1-benzothiophen-3-yl)acetate (151.2 mg) and (2-methyl-6-(trifluoromethyl)pyridin-3-yl)methanol (112 mg) and THF (5.0 mL) was added ADDP (423 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 (EtOAc/hexane) to give the title compound (165 mg). 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-1e738883315041b88013efca891d1d98 |
| Source note | uspto-grants-2016_01 |