関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Bromo-4-isopropylbenzene | HCID 11462 | — |
| 反応物 | 2-Amino-4,5-dimethoxybenzonitrile | HCID 735967 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Ether tetrahydrofuran | HCID 21868444 | — |
| 生成物 | (2-Amino-4,5-dimethoxy-phenyl)-(4-isopropyl-phenyl)-methanone | HCID 59259172 | — |
反応手順
18.8 ml (30 mmol) of BuLi (1.6 M in hexane) is added dropwise to a cooled (−5° C.) solution of 6 g (30 mmol) 4-isopropyl-1-bromobenzene in 25 ml ether. The reaction mixture is stirred for 15 min at −5° C. and one additional hour at rt. After that time the solution is cooled to −5° C. and a solution 1.8 g (10 mmol) 2-amino-4,5-dimethoxybenzonitrile in 20 ml ether/THF (1:1) is added dropwise. After 30 min the reaction mixture is poured slowly into water and extracted with ethyl acetate. The organic layer is dried and evaporated. The crude material is dissolved in 200 ml ether and stirred with 100 ml 2N HCl for one hour. After chromatography (DCM/MeOH 15:1) the product is obtained as yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08476286B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-3953030811ec4672bfe2eb375b1b9c64 |
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| 出典メモ | uspto-grants-2013_07 |
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