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 | 5-Bromo-2-methyl-1-benzothiophene | HCID 13663035 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 5-Bromo-2-(bromomethyl)benzo[b]thiophene | HCID 14819352 | 90.1% |
反応手順
According to the procedure of S. Gronowitz, et al., Synth. Commin., 6, (7), 475 (1976), to a stirred, boiling partial solution of N-bromosuccinimide (17.63 g, 0.099 mol) in CCl4 (200 mL) was added 2,2'-azobis-(2-methylpropionitrile) (1.1 g, 0.007 mol). After one minute, a solution of 5-bromo-2-methylbenzthiophene (15.0 g, 0.066 mol) in CCl4 (100 mL) was added. The resulting mixture was heated at reflux for 2 hours and cooled to 0° C. The solid was filtered. The filtrate was concentrated to give 18.19 g (90%) of product as an orange solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04895860 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-b90f1f9bb09e477b8e1100f37d3a4b81 |
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| 出典メモ | uspto-grants-1990_01 |
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