Hydrochloric Acid → 1H-Imidazole-1-ethanol, 5-((3,5-dichlorophenyl)thio)-2-(hydroxymethyl)-4-(1-methylethyl)-

HRID 1857755노트

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HRID 1857755 반응식
Cl.C([O:9][CH2:10][C:11]1[N:12]([CH2:28][CH2:29][OH:30])[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:27][C:22]1[CH:21]=[C:20]([S:19][C:13]2[N:12]([CH2:28][CH2:29][OH:30])[C:11]([CH2:10][OH:9])=[N:15][C:14]=2[CH:16]([CH3:18])[CH3:17])[CH:25]=[C:24]([Cl:26])[CH:23]=1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 4740901H-Imidazole-1-ethanol, 5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-2-((phenylmethoxy)methyl)-HCID 516892Sodium Bicarbonate

생성물 1

HCID 4740911H-Imidazole-1-ethanol, 5-((3,5-dichlorophenyl)thio)-2-(hydroxymethyl)-4-(1-methylethyl)-수율 67%

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온도
110 °C

실험 절차

Added was 18 ml of cocentrated hydrochloric acid to 1.8 g (4.0 mmol) of the alcohol compound (118c), and the mixture was stirred with heating at 110° C. for 7 hours. After cooling, 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 (ethyl acetate) to give 960 mg of 2-(5-(3,5-dichlorophenyl-thio)-2-hydroxymethyl-4-isopropyl-1H-imidazol-1-yl)ethanol (119b) as oil (yield 67%).

후처리

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

출처 및 근거

ORD 기록
ord-f56d041f5b474689aac9aed1bf232bbf
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06147097

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