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Hydrochloric Acid → [1-Benzyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1H-imidazol-2-yl]methanol

HRID 1415998
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HRID 1415998 반응식
[CH2:1]([N:8]1[C:12]([S:13][C:14]2[CH:19]=[C:18]([Cl:20])[CH:17]=[C:16]([Cl:21])[CH:15]=2)=[C:11]([CH:22]([CH3:24])[CH3:23])[N:10]=[C:9]1[CH2:25][O:26]CC1C=CC(OC)=CC=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>CO>[CH2:1]([N:8]1[C:12]([S:13][C:14]2[CH:19]=[C:18]([Cl:20])[CH:17]=[C:16]([Cl:21])[CH:15]=2)=[C:11]([CH:22]([CH3:24])[CH3:23])[N:10]=[C:9]1[CH2:25][OH:26])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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4

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HCID 313Hydrochloric AcidHCID 221309361-benzyl-5-(3,5-dichlorophenylthio)-4-isopropyl-2-(p-methoxybenzyloxymethyl)-1H-imidazole

생성물 1

HCID 473924[1-Benzyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1H-imidazol-2-yl]methanol수율 92%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

To 25 ml of methanol was dissolved 1.41 g (2.67 mmol)of 1-benzyl-5-(3,5-dichlorophenylthio )-4-isopropyl-2-(p-methoxybenzyloxymethyl)-1H-imidazole (17f), followed by addition of 12.5 ml of 6N-hydrochloric acid at room temperature with stirring, and the mixture was stirred under heating at 60° C. for 3 hour. This reaction mixture was concentrated under reduced pressure, the residual solution was neutralized with a saturated aqueous solution of sodium bicarbonate to be weakly basic, and was extracted with methylene chloride. The extract was rinsed with water, and then, was dried over magnesium sulfate, and the solvent was concentrated under reduced pressure. The residue was crystalized from n-hexane and collected by filtration to give 1.0 g (yield 92%)of [1-benzyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1H-imidazol-2-yl]methanol (Compound I-16). mp 121-124° C.

후처리

  1. stirringthe mixture was stirred
  2. concentrationThis reaction mixture was concentrated under reduced pressure
  3. extractionwas extracted with methylene chloride
  4. washThe extract was rinsed with water
  5. dry with materialwas dried over magnesium sulfate
  6. concentrationthe solvent was concentrated under reduced pressure
  7. customThe residue was crystalized from n-hexane
  8. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-6771b1bedb7b45c5a29adf2cd0f62caa
출처 데이터셋
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05910506

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