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Hydrochloric Acid → (2-Chloro-4-methanesulfonyl-phenyl)-methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Chloro-4-(methylsulfonyl)benzaldehyde | HCID 2761084 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (2-Chloro-4-methanesulfonyl-phenyl)-methanol | HCID 42609245 | — |
反応手順
To a stirred dispersion of 2-chloro-4-methanesulfonyl-benzaldehyde (25 g, 0.11 mol) in absolute ethanol (120 ml) is added sodium borohydride (4.6 g, 0.12 mol) whilst cooling with an ice-bath to maintain room temperature. After stirring at room temperature for 3 hours, the reaction mixture is poured carefully onto ice-water (600 ml) and acidified to pH 1-2 with 1N HCl. The resulting suspension is extracted with ethyl acetate (400 ml) and the organic portions are combined, washed with brine, dried (MgSO4) and concentrated in vacuo. The resulting crude product is dried in a vacuum oven at 40° C. overnight to yield the titled product which is used crude in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07666878B2 |
| 出典データセット | uspto-grants-2010_02 |
| ORD ID | ord-1be371a3ba1643f88ed967bcafcc8c96 |
| 出典メモ | uspto-grants-2010_02 |