反応式
[H-].[Na+].[CH3:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[CH2:11][CH2:12][CH2:13][CH2:14][OH:15].[Br:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22]Br.O>C1COCC1>[Br:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][O:15][CH2:14][CH2:13][CH2:12][CH2:11][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=1[O:4][CH3:3]参加物
6
実験手順
NaH (46% dispersion in oil; 1.36 g) was added portionwise to a solution of 2-methoxybenzenbutanol (5.0 g) and 1,6-dibromohexane (1.38 g) in THF (50 ml). The suspension was refluxed for 20 h and was treated cautiously with H2O (20 ml). The resulting emulsion was extracted with ER (2×50 ml) and the dried extract was evaporated to leave a yellow oil. The oil was purified on a column of silica (Merck 5385, 600 ml) [A] to give the title compound as a colorless oil (5.6 g). T.l.c. [B] Rf 0.2.
後処理
- temperatureThe suspension was refluxed for 20 h
- extractionThe resulting emulsion was extracted with ER (2×50 ml)
- extractionthe dried extract
- customwas evaporated
- customto leave a yellow oil
- customThe oil was purified on a column of silica (Merck 5385, 600 ml) [A]
出典と根拠
- ORDレコード
- ord-ec67bbcf84b14f1a92bbdc820fa01aff
- 出典データセット
- uspto-grants-1992_06
- 特許番号
- US05126375
関連ノート
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