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1-Methylimidazole → 4-(1-(Bis(4-methoxyphenyl)(phenyl)methoxy)icosan-3-yloxy)-4-oxobutanoic acid triethylamine salt

HRID 1886893
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HRID 1886893 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([C:38]2[CH:43]=[CH:42][C:41]([O:44][CH3:45])=[CH:40][CH:39]=2)([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[O:10][CH2:11][CH2:12][CH:13]([OH:31])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:5][CH:4]=1.[C:46]1(=[O:52])[O:51][C:49](=[O:50])[CH2:48][CH2:47]1.[CH2:53]([N:55]([CH2:58][CH3:59])[CH2:56][CH3:57])[CH3:54].CN1C=CN=C1>C(Cl)Cl>[CH2:53]([N:55]([CH2:58][CH3:59])[CH2:56][CH3:57])[CH3:54].[CH3:45][O:44][C:41]1[CH:40]=[CH:39][C:38]([C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[O:10][CH2:11][CH2:12][CH:13]([O:31][C:46](=[O:52])[CH2:47][CH2:48][C:49]([OH:51])=[O:50])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:43][CH:42]=1
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참가 물질

6

반응물 4

HCID 13901-MethylimidazoleHCID 7922Succinic anhydrideHCID 8471TriethylamineHCID 687487641-(Bis(4-methoxyphenyl)(phenyl)methoxy)icosan-3-ol

생성물 1

HCID 687468894-(1-(Bis(4-methoxyphenyl)(phenyl)methoxy)icosan-3-yloxy)-4-oxobutanoic acid triethylamine salt

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
2회

실험 절차

1-(bis(4-methoxyphenyl)(phenyl)methoxy)icosan-3-ol (6.8 g, 11.0 mmoles), succinic anhydride (1.1 g, 11.0 mmoles), triethylamine (4.6 mL, 33.0 mmoles) and 1-methylimidazole (0.44 mL, 5.5 mmoles) are dissolved in methylene chloride (68 mL). The reaction is stirred at ambient temperature for five days, during which time the solution darkened. The solution is then diluted with methylene chloride (100 mL) and washed twice with ice-cold aqueous citric acid (10% [w/v], 50 mL) and once with saturated aqueous sodium chloride (50 mL). The methylene chloride solution is dried over anhydrous sodium sulfate, filtered and evaporated to a dark resin. The crude product is purified on silica gel (200 mL bed volume) eluting with methylene chloride:triethylamine (95:5 [v/v/v], 500 mL), then methylene chloride:methanol:triethylamine (93:2:5 [v/v/v], 1000 mL). Fractions containing pure product by thin layer chromatography are pooled and evaporated to a resin. The resin is dried well in vacuo. The yield is 2.4 g (30%).

후처리

  1. washwashed twice with ice-cold aqueous citric acid (10% [w/v], 50 mL) and once with saturated aqueous sodium chloride (50 mL)
  2. dry with materialThe methylene chloride solution is dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. customevaporated to a dark resin
  5. customThe crude product is purified on silica gel (200 mL bed volume)
  6. washeluting with methylene chloride:triethylamine (95:5 [v/v/v], 500 mL)
  7. additionFractions containing pure product by thin layer chromatography
  8. customevaporated to a resin
  9. customThe resin is dried well in vacuo

출처 및 근거

ORD 기록
ord-ddd8ad3cc9354c3692719c4d2c851518
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08501706B2

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