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

HRID 1257468
ノート
印刷プレビュー

反応式

HRID 1257468 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-c473dceb8fd7411ea76de55e39e8dcef
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461348B2

反応ノート

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