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Tributylphosphine → Methyl(4-methyl-6-((2-methyl-6-(trifluoromethyl)pyridin-3-yl)methoxy)-1-benzothiophen-3-yl)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tributylphosphine | HCID 13831 | — |
| 反応物 | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| 反応物 | (2-Methyl-6-(trifluoromethyl)pyridin-3-yl)methanol | HCID 2760122 | — |
| 反応物 | Methyl(6-hydroxy-4-methyl-1-benzothiophen-3-yl)acetate | HCID 121001301 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl(4-methyl-6-((2-methyl-6-(trifluoromethyl)pyridin-3-yl)methoxy)-1-benzothiophen-3-yl)acetate | HCID 89775295 | 91.6% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09238639B2 |
| 出典データセット | uspto-grants-2016_01 |
| ORD ID | ord-8bfb848d220d41678cd37a795211d878 |
| 出典メモ | uspto-grants-2016_01 |