関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoyl Peroxide | HCID 7187 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 2-Chloro-3-methylbenzoic acid | HCID 139879 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-(Bromomethyl)-2-chlorobenzoic acid | HCID 20221490 | — |
反応手順
Benzoyl peroxide (1.33 g) was added to a suspension of 2-chloro-3-methylbenzoic acid (25 g) and N-bromosuccinimide (28.7 g) in chlorobenzene (250 mL) and the resulting mixture was heated to 85° C. for 4 h. The mixture was diluted with ethyl acetate (100 mL) and washed with 10% aqueous brine (3×100 mL). The organic layer was dried over magnesium sulphate, filtered and evaporated. The beige solid was recrystallised from ethyl acetate (˜75 mL)/isohexane (˜250 mL) to give the subtitled compound as a white solid. Yield 25.3 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08476265B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-336c9319b0a741feb0a495d2b211fae1 |
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| 出典メモ | uspto-grants-2013_07 |
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