Pyridinium chloride → 1-(2'-Ethyl-5'-hydroxy-2-propylbiphenyl-4-yl)-1-propanone

HRID 1869726ノート

反応式

HRID 1869726 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([O:9]C)=[CH:5][C:4]=1[C:11]1[CH:16]=[CH:15][C:14]([C:17](=[O:20])[CH2:18][CH3:19])=[CH:13][C:12]=1[CH2:21][CH2:22][CH3:23])[CH3:2].Cl.N1C=CC=CC=1>O>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][C:4]=1[C:11]1[CH:16]=[CH:15][C:14]([C:17](=[O:20])[CH2:18][CH3:19])=[CH:13][C:12]=1[CH2:21][CH2:22][CH3:23])[CH3:2]

参加物

4

反応物 2

HCID 10176127Pyridinium chlorideHCID 668792591-(2'-Ethyl-5'-methoxy-2-propylbiphenyl-4-yl)propan-1-one

生成物 1

HCID 223456391-(2'-Ethyl-5'-hydroxy-2-propylbiphenyl-4-yl)-1-propanone

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
30 °C

実験手順

413 g (1.33 mol) of 1-(2′-ethyl-5′-methoxy-2-propylbiphenyl-4-yl)propan-1-one and 768 g (6.64 mol) of pyridine hydrochloride are placed in a round-bottomed flask. The mixture is heated at 160°-170° C. for 4 hours with stirring. The reaction medium is allowed to return to 100°-110° C. and 800 ml of water are added. The mixture is cooled to 30° C. and extracted with 1.6 liters of ethyl acetate. After separating by settling, the aqueous phase is extracted with 600 ml of ethyl acetate. The organic phases are combined and washed twice with 800 ml of water. After evaporating under reduced vacuum, 410 g of 1-(2′-ethyl-5′-hydroxy-2-propylbiphenyl-4-yl)propan-1-one are obtained in the form of an oil.

後処理

  1. temperatureThe mixture is heated at 160°-170° C. for 4 hours
  2. customto return to 100°-110° C.
  3. extractionextracted with 1.6 liters of ethyl acetate
  4. customAfter separating
  5. extractionthe aqueous phase is extracted with 600 ml of ethyl acetate
  6. washwashed twice with 800 ml of water
  7. customAfter evaporating under reduced vacuum, 410 g of 1-(2′-ethyl-5′-hydroxy-2-propylbiphenyl-4-yl)propan-1-one
  8. customare obtained in the form of an oil

出典と根拠

ORDレコード
ord-b1fbc9cd125b4ec9b0e327045166c247
出典データセット
uspto-grants-2009_12
特許番号
US07638657B2

反応ノート

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