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Water → 5-Chloro-alpha-(2-chlorophenyl)-2-(2,4-dimethoxybenzyl)aminobenzyl alcohol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2,4-Dimethoxybenzaldehyde | HCID 69175 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | (2-Amino-5-chlorophenyl)(2-chlorophenyl)methanol | HCID 11437092 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-Chloro-alpha-(2-chlorophenyl)-2-(2,4-dimethoxybenzyl)aminobenzyl alcohol | HCID 53841495 | 96.1% |
反応手順
To a solution of 2-amino-5-chloro-α-(2-chloro phenyl)benzyl alcohol (5.0 g) and 2,4-dimethoxy benzaldehyde (3.72 g) in acetic acid (50 ml) was added, under ice-cooling, sodium borohydride (0.94 g). The mixture was stirred for one hour at room temperature, which was poured into water (200 ml), followed by extraction with ethyl acetate (200 ml×2). The ethyl acetate layer was washed with 1N sodium hydroxide, which was dried over anhydrous magnesium sulfate, followed by distilling off the solvent under reduced pressure. The residue was purified by means of a silica gel column chromatography (hexane:ethyl acetate=5:1) to give 5-chloro-α-(2-chlorophenyl)-2-(2,4-dimethoxybenzyl)aminobenzyl alcohol (7.5 g) as an oily product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726306 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-8208d819f879448fbecf7d2aa5f1ad04 |
| 出典メモ | uspto-grants-1998_03 |