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

HRID 1869726노트

반응식

HRID 1869726 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
30 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b1fbc9cd125b4ec9b0e327045166c247
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07638657B2

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