化工社化工社 化学情報印刷レポート · 研究参考用
Azobisisobutyronitrile → 6-Bromo-7-(bromomethyl)-1,1,4,4-tetramethyl-1,2,3,4-tetrahydronaphthalene
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 | 6-Bromo-1,1,4,4,7-pentamethyl-1,2,3,4-tetrahydronaphthalene | HCID 10039346 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 6-Bromo-7-(bromomethyl)-1,1,4,4-tetramethyl-1,2,3,4-tetrahydronaphthalene | HCID 23498953 | — |
反応手順
The mixture of 6-bromo-7-methyl-1,1,4,4-tetramethyl-1,2,3,4-tetrahydronaphthalene (4.20 g, 15 mmol), NBS (3.20 g, 18 mmol), 2,2′-azobisisobutyronitrile (0.3 g, 1.8 mmol) and CCl4 (120 mL) was heated at reflux for 16 hours. The mixture was concentrated under reduced pressure to about 50 mL. The reaction was then filtered, and the solid was washed with Et2O (20 mL). The combined organic solution was then concentrated under vacuum to generate crude product. Crude 91.2 was generated as a brown oil and used directly in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07582803B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-4d9162968f024969a493a6db5ba91605 |
| 出典メモ | uspto-grants-2009_09 |