Potassium Iodide → HCID 20227255、化合物

HRID 1731813ノート

反応式

HRID 1731813 の反応式
Cl[CH2:2][C:3](=[O:5])[CH3:4].[Br:6][C:7]1[C:8]([OH:17])=[C:9]([N+:14]([O-:16])=[O:15])[CH:10]=[CH:11][C:12]=1[F:13].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CC(C)=O>[Br:6][C:7]1[C:12]([F:13])=[CH:11][CH:10]=[C:9]([N+:14]([O-:16])=[O:15])[C:8]=1[O:17][CH2:2][C:3](=[O:5])[CH3:4]

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 6571ChloroacetoneHCID 11430Potassium CarbonateHCID 137328542-Bromo-3-fluoro-6-nitrophenol

生成物 1

HCID 20227255HCID 20227255、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Chloroacetone (3.8 g, 3.3 ml, 41 mmol) was added dropwise to a solution of 3-bromo-4-fluoro-2-hydroxy-1-nitrobenzene (4.3 g, 18.2 mmol) in acetone (54 ml) with stirring at ambient temperature. Potassium carbonate (5.8 g, 42 mmol) and potassium iodide (6.0 g, 36.4 mmol), were added and the reaction mixture was heated to reflux temperature for 2 hours. The reaction mixture was then cooled to room temperature, poured onto water (100 ml), and extracted three times with ethyl acetate (150 ml). The combined organic layers were dried over magnesium sulfate, treated with decolorizing charcoal and filtered through diatomaceous earth. Solvent was removed in vacuo to afford a dark brown oil.

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux temperature for 2 hours
  3. temperatureThe reaction mixture was then cooled to room temperature
  4. additionpoured onto water (100 ml)
  5. extractionextracted three times with ethyl acetate (150 ml)
  6. dry with materialThe combined organic layers were dried over magnesium sulfate
  7. additiontreated with decolorizing charcoal
  8. filtrationfiltered through diatomaceous earth
  9. customSolvent was removed in vacuo
  10. customto afford a dark brown oil

出典と根拠

ORDレコード
ord-b5b5d443f0944165b5c2bde93a10cdc1
出典データセット
uspto-grants-1986_11
特許番号
US04623650

反応ノート

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