Ethyl formate → alpha-Formyl-4-benzylphenylacetonitrile
反応式
C[O-].[Na+].[CH:4](OCC)=[O:5].[CH2:9]([C:16]1[CH:21]=[CH:20][C:19]([CH2:22][C:23]#[N:24])=[CH:18][CH:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>C1(C)C=CC=CC=1>[CH:4]([CH:22]([C:19]1[CH:18]=[CH:17][C:16]([CH2:9][C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)=[CH:21][CH:20]=1)[C:23]#[N:24])=[O:5]参加物
5
実験手順
To a suspention of sodium methoxide (64.26 g) in toluene (2.5 l) was added dropwise at 0° C. a mixture of ethyl formate (88.14 g) and 4-benzylphenylacetonitrile (189.69 g) with stirring. After 30 minutes, ice bath was removed. After 20 hours, ice water (2.6 l) was added to the reaction mixture, and the aqueous layer was separated. The organic layer was washed with 0.5N sodium hydroxide aqueous solution (500 ml×5). The aqueous layer and the washings were combined, adjusted to acid with conc. hydrochloric acid, and stirred at 0° C. for 30 minutes. The precipitate was separated by filtration, washed, and dried to give the title compound.(152.22 g).
後処理
- customice bath was removed
- waitAfter 20 hours
- additionice water (2.6 l) was added to the reaction mixture
- customthe aqueous layer was separated
- washThe organic layer was washed with 0.5N sodium hydroxide aqueous solution (500 ml×5)
- stirringstirred at 0° C. for 30 minutes
- customThe precipitate was separated by filtration
- washwashed
- customdried
出典と根拠
- ORDレコード
- ord-24c264f70b1c409e990b7a11db3879ef
- 出典データセット
- uspto-grants-1995_04
- 特許番号
- US05409928
反応ノート
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