Pyridine → HCID 13627682, 화합물

HRID 1789086노트

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HRID 1789086 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][CH3:16])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[CH2:17]([O:22][C:23]1[CH:28]=[CH:27][C:26]([CH2:29][CH2:30][C:31](Cl)=[O:32])=[CH:25][CH:24]=1)[CH2:18][CH2:19][CH2:20][CH3:21].N1C=CC=C[CH:35]=1>O>[CH3:35][CH:30]([CH2:29][C:26]1[CH:27]=[CH:28][C:23]([O:22][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])=[CH:24][CH:25]=1)[C:31]([O:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][CH3:16])=[CH:10][CH:9]=2)=[CH:6][CH:7]=1)=[O:32]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 136276804-(4-n-Propylphenyl)phenolHCID 53826862HCID 53826862, 화합물

생성물 1

HCID 13627682HCID 13627682, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4-Hydroxy-4'-propylbiphenyl (2.5 g, 0.012 mol) was dissolved in pyridine (10 ml) and to the solution was added β-(4-pentyloxyphenyl)propionic acid chloride (2.5 g, 0.01 mol) with sufficient shaking, followed by allowing the resulting reaction solution to stand overnight, pouring it in water (100 ml), extracting the resulting oily material with toluene (100 ml), washing the toluene layer with 6N-HCl, then with 2N-NaOH and further with water till the washing water became neutral, filtering, distilling off toluene under reduced pressure, and recrystallizing residual crystals from ethanol to obtain the objective 4'-propyl-4-biphenylyl α-methyl-β-(4-pentyloxyphenyl)propionate. m.p. 84.0°-84.5° C. N-I point 46.0° C. (extrapolated value).

후처리

  1. customthe resulting reaction solution
  2. extractionextracting the resulting oily material with toluene (100 ml)
  3. washwashing the toluene layer with 6N-HCl
  4. filtrationfiltering
  5. distillationdistilling off toluene under reduced pressure
  6. customrecrystallizing residual crystals from ethanol

출처 및 근거

ORD 기록
ord-149cf621368447ca9478e75c0d11594b
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04686305

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