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Water → 4-(Iodomethyl)-2-[3-(trifluoromethyl)phenyl]-1,3-thiazole

HRID 1257468
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HRID 1257468 반응식
Cl[CH2:2][C:3]1[N:4]=[C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=2)[S:6][CH:7]=1.[I-:18].[Na+].O>CC(C)=O>[I:18][CH2:2][C:3]1[N:4]=[C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=2)[S:6][CH:7]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 5238Sodium IodideHCID 150453854-(Chloromethyl)-2-[3-(trifluoromethyl)phenyl]-1,3-thiazole

생성물 1

HCID 669395234-(Iodomethyl)-2-[3-(trifluoromethyl)phenyl]-1,3-thiazole수율 28%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution (10 mL) of the compound (1.0 g, 3.6 mmol) obtained in Example 21a in acetone was added sodium iodide (1.6 g, 11 mmol), and the mixture was stirred at room temperature overnight. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The resulting crude title compound was purified by column chromatography (hexane-hexane/ethyl acetate=70/30) to give the title compound (370 mg, 28%) as a colorless solid.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe obtained organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customThe resulting crude title compound was purified by column chromatography (hexane-hexane/ethyl acetate=70/30)

출처 및 근거

ORD 기록
ord-c473dceb8fd7411ea76de55e39e8dcef
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461348B2

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