Aluminium lithium hydride → 4-(Difluoromethyl)benzenemethanol
反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[F:7][CH:8]([F:19])[C:9]1[CH:18]=[CH:17][C:12]([C:13](OC)=[O:14])=[CH:11][CH:10]=1>C1COCC1>[F:7][CH:8]([F:19])[C:9]1[CH:10]=[CH:11][C:12]([CH2:13][OH:14])=[CH:17][CH:18]=1参加物
4
実験手順
A solution of LAH (1.0 M in THF, 31 mL, 31 mmol) was added dropwise to a solution of Example 38A (5.82 g, 31.3 mmol) in THF (100 mL) at 0° C. The reaction was stirred for 1 hr, then quenched by careful addition of solid Na2SO4.10H2O. The mixture was warmed to ambient temperature and stirred 30 min. Celite filter aid was added and the mixture was filtered. The filtrate was concentrated in vacuo to yield 4.02 g (81%) of the title compound as a colorless oil. 1H NMR (300 MHz, DMSO-d6) δ 7.52 (d, J=8.2, 2H), 7.48-7.41 (m, 2H), 7.00 (t, J=56.0, 1H), 5.30 (t, J=5.7, 1H), 4.55 (d, J=5.4, 2H).
後処理
- customquenched by careful addition of solid Na2SO4.10H2O
- stirringstirred 30 min
- filtrationCelite filter aid
- additionwas added
- filtrationthe mixture was filtered
- concentrationThe filtrate was concentrated in vacuo
出典と根拠
- ORDレコード
- ord-84fa6256da5a4113b37a983f18ad73fb
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07998993B2
反応ノート
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