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

HRID 2254969ノート

反応式

HRID 2254969 の反応式
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]

参加物

4

反応物 2

HCID 21899381Acetic acid--water (1/1)HCID 53784545HCID 53784545、化合物

生成物 1

HCID 54145672(4'-Cyano-4-biphenylyl)acetaldehyde収率 104.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-aa323b2ada284abe883750adb8b2994c
出典データセット
uspto-grants-1993_08
特許番号
US05238602

反応ノート

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