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N-Iodosuccinimide → 1-(5-Chloro-4-fluoro-2-hydroxy-3-iodophenyl)ethanone

HRID 510942
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HRID 510942 반응식
[Cl:1][C:2]1[C:3]([F:12])=[CH:4][C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1.[I:13]N1C(=O)CCC1=O>C(O)(=O)C>[Cl:1][C:2]1[C:3]([F:12])=[C:4]([I:13])[C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1
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참가 물질

4

반응물 2

HCID 120273N-IodosuccinimideHCID 162214361-(5-Chloro-4-fluoro-2-hydroxyphenyl)ethanone

생성물 1

HCID 866668571-(5-Chloro-4-fluoro-2-hydroxy-3-iodophenyl)ethanone

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
70 °C

실험 절차

A solution of 1-(5-chloro-4-fluoro-2-hydroxyphenyl)ethanone (23.8 g, 126 mmol) in acetic acid (100 mL) was treated with N-iodosuccinimide (34.1 g, 151 mmol) and stirred at 70° C. for 2 hours. The reaction mixture was concentrated, diluted with EtOAc and quenched with sat. NaHCO3 solution. The organic layer was separated, washed with water, dried over MgSO4 and concentrated under reduced pressure to give the desired product to be used in the next step without further purification.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with EtOAc
  3. customquenched with sat. NaHCO3 solution
  4. customThe organic layer was separated
  5. washwashed with water
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8fcb8817adc1452aba252d85dc052234
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096600B2

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