3-Pyridinecarboxaldehyde → 3-(3-Pyridinyl)-2-propenenitrile
反応式
C(OP([CH2:9][C:10]#[N:11])(=O)OCC)C.[N:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH:18]=O)[CH:13]=1>C1(C)C=CC=CC=1>[N:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH:18]=[CH:9][C:10]#[N:11])[CH:13]=1参加物
4
実験手順
95 ml (0.60 mol) of cyanomethylphosphonic acid diethyl ester and 50 ml (0.55 mol) of pyridine-3-carbaldehyde are dissolved in 1 L of toluene and mixed with 55 g (0.55 mol) of KHCO3. The mixture is heated for 1 hour in a preheated oil bath. The cooled mixture is mixed with additional toluene and washed with 1M NaHCO3, twice with water and with saturated common salt solution. The organic phase is dried and concentrated by evaporation in a vacuum. The residue is recrystallized from ethyl acetate/hexane, and 49.5 g (69%) of product is obtained. Melting point 99.5-101° C.
後処理
- temperatureThe mixture is heated for 1 hour in a preheated oil bath
- washwashed with 1M NaHCO3, twice with water and with saturated common salt solution
- customThe organic phase is dried
- concentrationconcentrated by evaporation in a vacuum
- customThe residue is recrystallized from ethyl acetate/hexane
出典と根拠
- ORDレコード
- ord-9b32bfbfa3d54b59838abd9c04d7dd00
- 出典データセット
- uspto-grants-2001_09
- 特許番号
- US06284779B1
反応ノート
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