反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[O:7]1[CH2:12][CH2:11][CH:10]([CH2:13][C:14](OCC)=[O:15])[CH2:9][CH2:8]1>O1CCCC1>[O:7]1[CH2:12][CH2:11][CH:10]([CH2:13][CH2:14][OH:15])[CH2:9][CH2:8]1参加物
4
実験手順
To 15 mL of tetrahydrofuran (THF) at 0° C. was added LiAlH4 (0.28 g, 7.3 mmol). This mixture was stirred for 10 min then the ethyl tetrahydropyran-4-yl-acetate (Combi-Blocks Inc., 0.50 g, 2.9 mmol) was added. The reaction was stirred for 5 min at 0° C. then was allowed to warm to ambient temperature and was stirred for 90 min. The reaction was quenched with excess NaHSO4.10H2O and was stirred for 60 min. The mixture was filtered through Celite. The filtrate was concentrated to give the title compound which was carried on without further purification. MS (DCI/NH3) m/z 131 (M+H)+.
後処理
- stirringThe reaction was stirred for 5 min at 0° C.
- stirringwas stirred for 90 min
- customThe reaction was quenched with excess NaHSO4.10H2O
- stirringwas stirred for 60 min
- filtrationThe mixture was filtered through Celite
- concentrationThe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-5976d4588e174b91ab708aed313d55d1
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07560481B2
関連ノート
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