関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 3,5-Difluoro-4-triisopropylsilanyloxybenzaldehyde | HCID 57971920 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1,3-Difluoro-5-hydroxymethyl-2-triisopropylsilanyloxybenzene | HCID 57971896 | — |
反応手順
35.0 g (111 mmol) of 3,5-difluoro-4-triisopropylsilanyloxybenzaldehyde are introduced into 150 ml of water and 40 ml of methanol, cooled to 0° C. and, after addition of 8.42 g (222 mmol) of sodium borohydride in portions, stirred at RT overnight. The mixture is cautiously acidified with 1 N hydrochloric acid and extracted with ethyl acetate, and the combined organic phases are washed with saturated sodium chloride solution and dried over magnesium sulfate, and the solvent is distilled out in vacuo. Chromatography on silica gel 60 (mobile phase: cyclohexane/ethyl acetate 4:1) results in 29.5 g (93.2 mmol, 84% of theory) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08173704B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-74494ef89d704db8a97c6cb4d099dcd0 |
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| 出典メモ | uspto-grants-2012_05 |
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