HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tributylphosphine → Methyl(4-methyl-6-((2-methyl-6-(trifluoromethyl)pyridin-3-yl)methoxy)-1-benzothiophen-3-yl)acetate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Tributylphosphine | HCID 13831 | — |
| Edukt | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Edukt | (2-Methyl-6-(trifluoromethyl)pyridin-3-yl)methanol | HCID 2760122 | — |
| Edukt | Methyl(6-hydroxy-4-methyl-1-benzothiophen-3-yl)acetate | HCID 121001301 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | Methyl(4-methyl-6-((2-methyl-6-(trifluoromethyl)pyridin-3-yl)methoxy)-1-benzothiophen-3-yl)acetate | HCID 89775295 | 91,6% |
Reaktionsschritte
To a mixture of methyl(6-hydroxy-4-methyl-1-benzothiophen-3-yl)acetate (150 mg) and THF (dry) (5 mL) were added (2-methyl-6-(trifluoromethyl)pyridin-3-yl)methanol (133 mg), tri-n-butylphosphine (0.204 mL) and ADDP (192 mg) at room temperature. The mixture was stirred at room temperature for 4 h. The insoluble material was removed by filtration, and the filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (238 mg).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09238639B2 |
| Quelldatensatz | uspto-grants-2016_01 |
| ORD ID | ord-8bfb848d220d41678cd37a795211d878 |
| Quellennotiz | uspto-grants-2016_01 |