関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzaldehyde | HCID 240 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | (3-Bromophenyl)acetonitrile | HCID 36023 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(3-Bromo-phenyl)-3-phenyl-propionitrile | HCID 59331981 | 52% |
反応手順
A solution of 40% KOH (2.83 g in 5.0 ml of H2O) in ethanol (13 ml) was added to a solution of benzaldehyde (2.85 ml, 28.05 mmol) and 3-bromophenylacetonitrile (5 g, 25.50 mmol) in ethanol (9 ml). The reaction mixture was then stirred at room temperature for 2 hours and the precipitate was collected by suction filtration and washed with cold ethanol (6.68 g, 92%). The crude product (3.45 g, 12.14 mmol) was then dissolved in ethanol (35 ml) and heated to 65° C. Sodium borohydride (459 mg, 12.14 mmol) was added in portions and the reaction mixture was maintained at this temperature for a further 2 hours. Upon cooling, water (10 ml) was added and the solvent was removed under reduced pressure. The residue was partitioned between water (100 ml) and ethyl acetate (100 ml). The organic layer was separated, dried (MgSO4), filtered and concentrated to afford the desired product (1.80 g, 52%), which was used without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541461B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-010974ad3b054543a18be438d0ff5066 |
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| 出典メモ | uspto-grants-2013_09 |
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