反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]2([CH3:13])[O:12][CH2:11][CH2:10][O:9]2)=[CH:4][CH:3]=1.[Li]CCCC.[CH:19](N1CCCCC1)=[O:20].Cl>C1COCC1>[CH:19]([C:2]1[CH:7]=[CH:6][C:5]([C:8]2([CH3:13])[O:12][CH2:11][CH2:10][O:9]2)=[CH:4][CH:3]=1)=[O:20]参加物
6
反応条件
- 温度
- 0 °C
実験手順
To a stirred solution of 2-(4-bromophenyl)-2-methyl-1,3-dioxolane (2.0 g, 8.23 mmol) in THF (7 ml) was added n-BuLi (1.61 M solution in hexane, 5.47 ml, 8.8 mmol) at −78° C. under nitrogen, and the mixture was stirred for 2 hour, then allowed to warm up to 0° C. for 30 min. A solution of 1-formylpiperidine (930 mg, 8.23 mmol) in THF (5 ml) was added, and the mixture was stirred for 2 hours. The mixture was made neutral by addition of 1N HCl solution, and the whole was extracted with diethylether. The organic layer was washed with saturated NaHCO3 aqueous solution, brine, dried over MgSO4, and concentrated in vacuo. The compound was used for next reaction without purification.
後処理
- stirringthe mixture was stirred for 2 hours
- extractionthe whole was extracted with diethylether
- washThe organic layer was washed with saturated NaHCO3 aqueous solution, brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe compound was used for next reaction without purification
出典と根拠
- ORDレコード
- ord-327ab84d4587430891d651c9838efa5f
- 出典データセット
- uspto-grants-2005_09
- 特許番号
- US06949536B2
関連ノート
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