関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 4-[(6-Chloro-2-fluoro-3-methylphenyl)oxy]-3-fluorobenzonitrile | HCID 68720989 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 4-{[3-(Bromomethyl)-6-chloro-2-fluorophenyl]oxy}-3-fluorobenzonitrile | HCID 68722621 | 52% |
反応手順
To a solution of 4-[(6-chloro-2-fluoro-3-methylphenyl)oxy]-3-fluorobenzonitrile (2.41 g, 8.62 mmol) and NBS (1.534 g, 8.62 mmol) in carbon tetrachloride (150 ml) was added AIBN (1.415 g, 8.62 mmol) and the reaction mixture was stirred at 80° C. overnight. The solvent was removed and the crude material was purified via silica gel chromatography to give 4-{[3-(bromomethyl)-6-chloro-2-fluorophenyl]oxy}-3-fluorobenzonitrile (1.60 g, 4.46 mmol, 52% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 8.08 (dd, 1H), 7.62 (d, 1H), 7.48-7.59 (m, 2H), 6.92 (t, 1H), 4.70 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08304419B2 |
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| 出典データセット | uspto-grants-2012_11 |
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| ORD ID | ord-239265706bd24a09b1a3b27b29ac51d4 |
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| 出典メモ | uspto-grants-2012_11 |
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