Acetic acid--water (1/1) → (4'-Cyano-4-biphenylyl)acetaldehyde

HRID 1731442노트

반응식

HRID 1731442 반응식
C[O:2][CH:3]=[CH:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][C:14]([C:17]#[N:18])=[CH:13][CH:12]=2)=[CH:7][CH:6]=1.C(O)(=O)C.O>O>[C:17]([C:14]1[CH:13]=[CH:12][C:11]([C:8]2[CH:9]=[CH:10][C:5]([CH2:4][CH:3]=[O:2])=[CH:6][CH:7]=2)=[CH:16][CH:15]=1)#[N:18]

참가 물질

4

반응 조건

온도
100 °C

실험 절차

A mixture of 4.9 g of 4'-(2-methoxyvinyl)-4-biphenylcarbonitrile and 80 ml of glacial acetic acid/water (vol. 2:1) was heated to reflux for 1.5 hours at 100° C. bath temperature. The reaction mixture was subsequently poured into 150 ml of water and extracted three times with 100 ml of methylene chloride each time. The organic phases were washed with 100 ml of water and with 100 ml of saturated sodium hydrogen carbonate solution, dried over magnesium sulphate and concentrated. There were obtained 4.8 g of (4'-cyano-4-biphenylyl)acetaldehyde as a yellowish, crystalline residue which was processed without additional purification; Rf-value (toluene/ethyl acetate vol. 90:10) 0.37.

후처리

  1. temperaturewas heated
  2. extractionextracted three times with 100 ml of methylene chloride each time
  3. washThe organic phases were washed with 100 ml of water and with 100 ml of saturated sodium hydrogen carbonate solution
  4. dry with materialdried over magnesium sulphate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2dc7e113ca55424185b73263a6e62dec
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04621901

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