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3-Nitrobenzaldehyde → 3-Nitrobenzyl alcohol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Nitrobenzaldehyde | HCID 7449 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Nitrobenzyl alcohol | HCID 69267 | 94.3% |
反応手順
To a solution of 3-nitrobenzaldehyde (1) (200 g, 1.32 mol) in methanol (1000 mL) at 0° C. under N2 atmosphere was slowly added NaBH4 (25 g, 0.66 mol) and then the reaction mixture was allowed to stir at room temperature for 1 h. The reaction mixture was re-cooled to 0° C. and quenched with ice-water, methanol was removed under reduced pressure and the residue was extracted with CH2Cl2 (5×200 mL). The combined organic layer was washed with brine, dried over anhydrous Na2SO4 and concentrated to furnish compound 2 (190.7 g, 93%) as liquid which was taken as such for next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07939556B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-c623c18fdc7a4d80828cab76ff0e972e |
| 出典メモ | uspto-grants-2011_05 |