反応式
[H-].[Na+].[CH3:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[C:5]=1[CH2:11][CH2:12][OH:13].[Br:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20]Br.O>C1COCC1>[Br:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][O:13][CH2:12][CH2:11][C:5]1[C:6]([CH3:10])=[CH:7][CH:8]=[CH:9][C:4]=1[CH3:3]参加物
6
実験手順
NaH (46% dispersion in oil; 4.2 g) was added portionwise to a solution of 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.
後処理
- temperatureThe mixture was refluxed for 18 h
- extractionThe resulting emulsion was extracted with ER (3×100 ml)
- extractionthe dried extract
- customwas evaporated
- customto leave a yellow oil
- customExcess 1,6-dibromohexane was removed under reduced pressure
- customthe residue was purified on a column of silica (300 ml) [B]
出典と根拠
- ORDレコード
- ord-1d30dff30bc74c148be6fa80ccee5c6a
- 出典データセット
- uspto-grants-1991_02
- 特許番号
- US04992474
関連ノート
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