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Imidazole → 4'-(6-((Tert-butyldimethylsilyl)oxy)hexyloxy)-4-biphenylcarboxylic acid

HRID 890904
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HRID 890904 반응식
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][C:18]([C:21]([OH:23])=[O:22])=[CH:17][CH:16]=2)=[CH:11][CH:10]=1.[Si:24](Cl)([C:27]([CH3:30])([CH3:29])[CH3:28])([CH3:26])[CH3:25].N1C=CN=C1.C([O-])([O-])=O.[K+].[K+]>CN(C)C=O.O1CCCC1.CO.O.C(OCC)C>[Si:24]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]=[CH:17][C:18]([C:21]([OH:23])=[O:22])=[CH:19][CH:20]=2)=[CH:11][CH:10]=1)([C:27]([CH3:30])([CH3:29])[CH3:28])([CH3:26])[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 4

HCID 795ImidazoleHCID 11430Potassium CarbonateHCID 28928tert-Butyldimethylsilyl chlorideHCID 222424974-(6-Hydroxyhexyloxy)biphenyl-4'-carboxylic acid

생성물 1

HCID 222424914'-(6-((Tert-butyldimethylsilyl)oxy)hexyloxy)-4-biphenylcarboxylic acid수율 99.5%

시약·촉매·용매 5

HCID 887
Methanol
용매
HCID 962Water용매
HCID 3283Diethyl Ether용매
HCID 6228Dimethylformamide용매
HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 9 (12.0 g, 38.22 mmol) and tert-butyldimethylsilyl chloride (13.07 g, 86.68 mmol) in anhydrous N,N-dimethylformamide (80 mL) was quickly added imidazole (10.62 g, 155.96 mmol). After stirring under argon overnight, the reaction mixture was shaken with diethyl ether (100 mL) and water (300 mL). The ethereal layer was separated and washed with a saturated NaHCO3 solution before drying over anhydrous MgSO4. The crude product resulting from evaporation of the solvent was purified by flash column chromatography on silica gel with methylene chloride: hexanes (1:1) as the eluent to afford a compound with silyl-protected hydroxyl and carboxyl groups. The compound was dissolved in tetrahydrofuran:methanol (120 mL:60 mL) followed by stirring with a solution of 10% K2CO3 aqueous solution (60 mL) for 1 h. The volume of the solution was reduced to 25% via evaporation under reduced pressure. Brine (250 ml; 120 g NaCl in 500 mL H2O) was added to the slurry, and the pH was adjusted to 5.0 with 1 M aqueous solution of potassium hydrogen sulfate, KHSO4. The precipitate was collected by filtration and washed with water followed by drying under vacuum at 70° C. to yield 10 (16.3 g, 99%). 1H NMR spectral data (400 MHz, Acetone-d6): δ 0.03 (s, 6H, —Si(CH3)2), δ 0.86 (s, 9H, —SiCCH3), δ 1.30–1.60 (m, 6H, —CH2—), δ 1.74 (m, 2H, —CH2—), δ 3.59 (t, 2H, —CH2OAr), δ 4.01 (t, 2H, SiOCH2—), δ7.03 (d, 2H, aromatic rings), δ 7.66 (d, 2H, aromatic rings), δ 7.70 (d, 2H, aromatic rings), δ 7.97 (d, 2H, aromatic rings).

후처리

  1. customThe ethereal layer was separated
  2. washwashed with a saturated NaHCO3 solution
  3. dry with materialbefore drying over anhydrous MgSO4
  4. customThe crude product resulting from evaporation of the solvent
  5. customwas purified by flash column chromatography on silica gel with methylene chloride: hexanes (1:1) as the eluent
  6. customto afford a compound with silyl-protected hydroxyl and carboxyl groups
  7. customThe volume of the solution was reduced to 25% via evaporation under reduced pressure
  8. additionBrine (250 ml; 120 g NaCl in 500 mL H2O) was added to the slurry
  9. filtrationThe precipitate was collected by filtration
  10. washwashed with water
  11. customby drying under vacuum at 70° C.

출처 및 근거

ORD 기록
ord-c850d5ceb8d6436d824b3ba5e5a81751
출처 데이터셋
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07001648B2

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