Acetyl chloride → 3-Iodophenyl acetate

HRID 985477노트

반응식

HRID 985477 반응식
[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]

참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 11430Potassium CarbonateHCID 122723-Iodophenol

생성물 1

HCID 131017693-Iodophenyl acetate수율 65%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-84b5c73554c140019667c1bce9a2e921
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06872730B2

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