関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 5-Chloro-2-(2,3-difluoro-6-methoxybenzyloxy)-4-nitroanisole | HCID 59309741 | — |
| 触媒 | Nickel(II) bromide | HCID 278492 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 59309639 | HCID 59309639 | 90.1% |
反応手順
To a mixture of 5-chloro-2-(2,3-difluoro-6-methoxybenzyloxy)-4-nitroanisole (9.41 g), nickel(II) bromide (0.29 g), tetrahydrofuran (100 mL) and methanol (100 mL) was added sodium borohydride (2.97 g) under ice-cooling, and the mixture was stirred under ice-cooling for 30 minutes, and then stirred at room temperature for 30 minutes. To the reaction mixture was added a saturated aqueous sodium hydrogen carbonate solution, and the resulting mixture was extracted with ethyl acetate. The extract was washed with brine twice, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=4/1-3/2) to give the title compound (7.77 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08217069B2 |
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| 出典データセット | uspto-grants-2012_07 |
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| ORD ID | ord-28cbfbd2958d4096bf3297721378fef3 |
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| 出典メモ | uspto-grants-2012_07 |
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