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Water → 2-[2-[(6-Bromohexyl)oxy]ethyl]-1,3-dimethylbenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,6-Dibromohexane | HCID 12368 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-(2,6-Dimethylphenyl)ethanol | HCID 33942 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-[2-[(6-Bromohexyl)oxy]ethyl]-1,3-dimethylbenzene | HCID 13375631 | 52.7% |
反応手順
NaH (46% dispersion in oil; 4.2 g) was added portionwise to a solution f 2,6-dimethylbenzenethanol (6.0 g) and 1,6-dibromohexane (19.52 g) in THF (50 ml) under nitrogen. The mixture was refluxed for 18 h and treated cautiously with H2O (20 ml). The resulting emulsion was extracted with ER (3×100 ml) and the dried extract was evaporated to leave a yellow oil. Excess 1,6-dibromohexane was removed under reduced pressure and the residue was purified on a column of silica (300 ml) [B] to give the title compound as a colourless oil (6.6 g) b.p. 110-115°/0.4 mmHg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05243076 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-acc0d0ac996740c1aa636be541a52c57 |
| 出典メモ | uspto-grants-1993_09 |