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Sodium Bicarbonate → [4-(3-Chlorophenyl)sulfanyl-5-isopropyl-1-methyl-imidazol-2-yl]methanol

HRID 1416006
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인쇄 미리보기

반응식

HRID 1416006 반응식
C([O:8][CH2:9][C:10]1[N:11]([CH3:26])[C:12]([CH:23]([CH3:25])[CH3:24])=[C:13]([S:15][C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([Cl:22])[CH:17]=2)[N:14]=1)C1C=CC=CC=1.C(=O)([O-])O.[Na+]>Cl>[Cl:22][C:18]1[CH:17]=[C:16]([S:15][C:13]2[N:14]=[C:10]([CH2:9][OH:8])[N:11]([CH3:26])[C:12]=2[CH:23]([CH3:25])[CH3:24])[CH:21]=[CH:20][CH:19]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 22130223HCID 22130223, 화합물

생성물 1

HCID 473947[4-(3-Chlorophenyl)sulfanyl-5-isopropyl-1-methyl-imidazol-2-yl]methanol수율 65%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
110 °C

실험 절차

In 5.8 ml of concented hydrochloric acid was dissolved 580 mg (1.5 mmol)of 2-benzyloxymethyl-4-(3-chlorophenylthio)-5-isopropyl-1-methyl-1H-imidazole (17ab'), and the mixture was refluxed under heating at 110° C. for 6 hours. The reaction mixture was neutralized with a saturated aqueous solution of sodium hydrogen carbonate, and extracted with methylene chloride. The organic layer was washed with water and dried over sodium sulfate, and the solvent was distilled off under reduced pressure. The crude product was recrystallized from ethyl acetate-isopropyl ether to give 289 mg of the objective Compound I-38 (yield 65%). mp 105-106° C.

후처리

  1. temperaturewas refluxed
  2. extractionextracted with methylene chloride
  3. washThe organic layer was washed with water
  4. dry with materialdried over sodium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe crude product was recrystallized from ethyl acetate-isopropyl ether

출처 및 근거

ORD 기록
ord-36d951b6f8984b4f93b0cfdecb4dcaea
출처 데이터셋
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05910506

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