HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tributylphosphine → Methyl(4,7-dichloro-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(4,7-dichloro-6-hydroxy-1-benzothiophen-3-yl)acetate | HCID 121006406 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | Methyl(4,7-dichloro-6-((2-methyl-6-(trifluoromethyl)pyridin-3-yl)methoxy)-1-benzothiophen-3-yl)acetate | HCID 118667007 | 73,4% |
Reaktionsschritte
To a mixture of tri-n-butylphosphine (0.336 mL), methyl(4,7-dichloro-6-hydroxy-1-benzothiophen-3-yl)acetate (130.7 mg), (2-methyl-6-(trifluoromethyl)pyridin-3-yl)methanol (94 mg) and THF (4.5 mL) was added ADDP (283 mg) at room temperature. The mixture was stirred at room temperature under nitrogen atmosphere overnight. The mixture was concentrated. To the residue was added IPE and the precipitate was filtered off. The filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (NH, EtOAc/hexane) to give the title compound (153 mg).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09238639B2 |
| Quelldatensatz | uspto-grants-2016_01 |
| ORD ID | ord-2f33e2f16840403784694e34b447ef39 |
| Quellennotiz | uspto-grants-2016_01 |