関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | 5-Chlorovaleryl chloride | HCID 74089 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Chloro-4,6-dimethylaniline | HCID 113033 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-Chloropentanoic acid (2-chloro-4,6-dimethylphenyl)amide | HCID 12143937 | — |
反応手順
To a solution of 2-chloro-4,6-dimethylaniline (14.7 g) and diisopropylethylamine (18 mL) in 150 mL of THF, was added a solution of 5-chlorovaleryl chloride (12.2 mL) in 75 mL of THF. After the reaction mixture had been allowed to stir at room temperature overnight, it was filtered and the filtrate concentrated on the rotary evaporator. The residue was dissolved in ethyl acetate and washed with 1 M aqueous HCl, saturated aqueous sodium bicarbonate, and brine. The ethyl acetate solution was then dried with magnesium sulfate and concentrated on the rotary evaporator to give a solid which was combined with a 1:1 mixture of hexane and diethyl ether. After this mixture had been stirred for an hour, it was filtered and the collected solids were dried to provide 12.2 g of 5-chloropentanoic acid (2-chloro-4,6-dimethylphenyl)amide, mp 80.6-82.9° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07268146B2 |
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| 出典データセット | uspto-grants-2007_09 |
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| ORD ID | ord-dad4dcf086f74905b22abda7b8b6fef1 |
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| 出典メモ | uspto-grants-2007_09 |
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