Hydrochloric Acid → (5-(3,5-Dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazol-2-yl)methanol

HRID 1415996

반응식

HRID 1415996 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([S:9][C:10]2[N:14]([CH3:15])[C:13]([CH2:16][O:17]CC3C=CC(OC)=CC=3)=[N:12][C:11]=2[CH:27]([CH3:29])[CH3:28])[CH:5]=[C:6]([Cl:8])[CH:7]=1.Cl>C(O)C>[Cl:8][C:6]1[CH:5]=[C:4]([S:9][C:10]2[N:14]([CH3:15])[C:13]([CH2:16][OH:17])=[N:12][C:11]=2[CH:27]([CH3:29])[CH3:28])[CH:3]=[C:2]([Cl:1])[CH:7]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 221305485-(3,5-dichlorophenylthio)-1-methyl-4-isopropyl-2-(p-methoxybenzyloxymethyl)-1H-imidazole

생성물 1

HCID 473916(5-(3,5-Dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazol-2-yl)methanol수율 95%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

(6)In 45 ml of ethanol was dissolved 9.10 g (20.1 mmol)of 5-(3,5-dichlorophenylthio)-1-methyl-4-isopropyl-2-(p-methoxybenzyloxymethyl)-1H-imidazole (17b), followed by addition of 90 ml of 6N-hydrochloric acid, and the mixture was refluxed for 1 hour. This reaction mixture was concentrated under reduced pressure to remove ethanol and the residue forming a couple of layers was extracted twice with n-hexane to remove p-methoxybenzyl chloride. The aqueous layer was extracted with methylene chloride and the extract was neutralized with an aqueous sodium bicarbonate solution and dried over magnesium sulfate. The solvent was then distilled off under reduced pressure and the residue was rinsed with isopropyl ether to provide 6.3 g (yield 95%)of [5-(3,5-dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazol-2-yl]methanol (12=Compound I-8). mp 157-158° C.

후처리

  1. temperaturethe mixture was refluxed for 1 hour
  2. concentrationThis reaction mixture was concentrated under reduced pressure
  3. customto remove ethanol
  4. customthe residue forming a couple of layers
  5. extractionwas extracted twice with n-hexane
  6. customto remove p-methoxybenzyl chloride
  7. extractionThe aqueous layer was extracted with methylene chloride
  8. dry with materialdried over magnesium sulfate
  9. distillationThe solvent was then distilled off under reduced pressure
  10. washthe residue was rinsed with isopropyl ether

출처 및 근거

ORD 기록
ord-3e204c1df2324d729b1f6e41b0f59f45
출처 데이터셋
uspto-grants-1999_06
특허 번호
US05910506

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