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

HRID 2254969노트

반응식

HRID 2254969 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

반응물 2

HCID 21899381Acetic acid--water (1/1)HCID 53784545HCID 53784545, 화합물

생성물 1

HCID 54145672(4'-Cyano-4-biphenylyl)acetaldehyde수율 104.2%

시약·촉매·용매 1

HCID 962Water용매

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-aa323b2ada284abe883750adb8b2994c
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05238602

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