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Pyridine, 4-((5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-2-(2-(phenylmethoxy)ethyl)-1H-imidazol-1-yl)methyl)- → 1H-Imidazole-2-ethanol, 5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-1-(4-pyridinylmethyl)-

HRID 1857758
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인쇄 미리보기

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HRID 1857758 반응식
C([O:8][CH2:9][CH2:10][C:11]1[N:12]([CH2:28][C:29]2[CH:34]=[CH:33][N:32]=[CH:31][CH:30]=2)[C:13]([S:19][C:20]2[CH:25]=[C:24]([Cl:26])[CH:23]=[C:22]([Cl:27])[CH:21]=2)=[C:14]([CH:16]([CH3:18])[CH3:17])[N:15]=1)C1C=CC=CC=1.C(=O)([O-])O.[Na+]>Cl>[Cl:26][C:24]1[CH:25]=[C:20]([S:19][C:13]2[N:12]([CH2:28][C:29]3[CH:34]=[CH:33][N:32]=[CH:31][CH:30]=3)[C:11]([CH2:10][CH2:9][OH:8])=[N:15][C:14]=2[CH:16]([CH3:18])[CH3:17])[CH:21]=[C:22]([Cl:27])[CH:23]=1
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4

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HCID 474064Pyridine, 4-((5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-2-(2-(phenylmethoxy)ethyl)-1H-imidazol-1-yl)methyl)-HCID 516892Sodium Bicarbonate

생성물 1

HCID 4740651H-Imidazole-2-ethanol, 5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-1-(4-pyridinylmethyl)-수율 67.3%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

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온도
100 °C

실험 절차

In 12 ml of cocentrated hydrochloric acid was dissolved 2.3 g (4.5 mmol) of the benzyl compound (122b), and the mixture was heated at 100° C. for 4 hours. The mixture was neutralized with sodium hydrogen carbonate, and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (7% methanol/ethyl acetate) to give 1.28 g of 2-[5-(3,5-dichlorophenylthio)-4-isopropyl-1-(pyridin-4-ylmethyl)-1H-imidazol-2-yl]ethanol (123b) as crystals (yield 67%). mp 121-122° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (7% methanol/ethyl acetate)

출처 및 근거

ORD 기록
ord-930a7d0a015847d195096d852802c1b3
출처 데이터셋
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06147097

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