3-Pyridinecarboxaldehyde → 3-(3-Pyridinyl)-2-propenenitrile
반응식
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]=1참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-9b32bfbfa3d54b59838abd9c04d7dd00
- 출처 데이터셋
- uspto-grants-2001_09
- 특허 번호
- US06284779B1
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