Hydrochloric Acid → 4-(2-Methyl-1,3-dioxolan-2-yl)benzaldehyde

HRID 497207

反応式

HRID 497207 の反応式
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

  1. stirringthe mixture was stirred for 2 hours
  2. extractionthe whole was extracted with diethylether
  3. washThe organic layer was washed with saturated NaHCO3 aqueous solution, brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. 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

読み込み中…