2,2-Dimethoxypropane → HCID 67356722、化合物

HRID 577827ノート

反応式

HRID 577827 の反応式
[F:1][C:2]1[C:9]([F:10])=[C:8]([F:11])C=C[C:3]=1[CH:4]=O.[CH3:12][O:13][C:14]([O:17][CH3:18])(C)[CH3:15]>CCOCC.CC1C=CC(S(O)(=O)=O)=CC=1>[CH3:12][O:13][CH:14]([O:17][CH3:18])[C:15]1[CH:4]=[CH:3][C:2]([F:1])=[C:9]([F:10])[C:8]=1[F:11]

参加物

5

反応物 2

HCID 64952,2-DimethoxypropaneHCID 5192262,3,4-Trifluorobenzaldehyde

生成物 1

HCID 67356722HCID 67356722、化合物収率 71.7%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 3283Diethyl Ether溶媒

実験手順

A solution of 2,3,4-trifluorobenzaldehyde (25 g, 156.16 mmol), 2,2-dimethoxypropane (58.1 ml, 468.48 mmol), and 4-methylbenzenesulfonic acid (0.269 g, 1.56 mmol) was stirred at room temperature overnight. The reaction mixture diluted with ether and washed successively with aq. sodium bicarbonate solution, water, and brine. The organic layer dried over sodium sulfate and concentrated. The residue was distilled under high vacuum to give the title compound (23.07 g, 71.7%).

後処理

  1. washwashed successively with aq. sodium bicarbonate solution, water, and brine
  2. dry with materialThe organic layer dried over sodium sulfate
  3. concentrationconcentrated
  4. distillationThe residue was distilled under high vacuum

出典と根拠

ORDレコード
ord-73668a9afa6d497f8d3d0788b8be06b6
出典データセット
uspto-grants-2015_05
特許番号
US09040528B2

反応ノート

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