Acetyl chloride → 3-Iodophenyl acetate

HRID 985477ノート

反応式

HRID 985477 の反応式
[I:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.[C:9](Cl)(=[O:11])[CH3:10].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[C:9]([O:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([I:1])[CH:3]=1)(=[O:11])[CH3:10]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 11430Potassium CarbonateHCID 122723-Iodophenol

生成物 1

HCID 131017693-Iodophenyl acetate収率 65%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3-iodophenol (3 g, 13.6 mmol), acetyl chloride (2.9 ml, 40.9 mmol) and potassium carbonate (9.42 g, 68.2 mmol) in N,N-dimethylformamide (75 ml) was stirred for 16 h at room temperature. The mixture was partitioned between water and ethyl acetate. The organic layer was washed with 1N NaOH, dried over magnesium sulfate, and evaporated under vacuum. The crude product was chromatographed over silica gel, eluting with 20% ethyl acetate/hexanes to yield 2.3 g (65%) of 3-iodophenyl acetate.

後処理

  1. customThe mixture was partitioned between water and ethyl acetate
  2. washThe organic layer was washed with 1N NaOH
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under vacuum
  5. customThe crude product was chromatographed over silica gel
  6. washeluting with 20% ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-84b5c73554c140019667c1bce9a2e921
出典データセット
uspto-grants-2005_03
特許番号
US06872730B2

反応ノート

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