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Iodine → 5-Bromo-4-formyl-2-methoxyphenyl acetate

HRID 1898759
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반응식

HRID 1898759 반응식
[C:1]([O:4][C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[O:10])=[CH:7][C:6]=1[O:13][CH3:14])(=[O:3])[CH3:2].C([O-])(=O)C.[Na+].II.[Br:22]Br>C(O)(=O)C.O>[C:1]([O:4][C:5]1[CH:12]=[C:11]([Br:22])[C:8]([CH:9]=[O:10])=[CH:7][C:6]=1[O:13][CH3:14])(=[O:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 807IodineHCID 24408BromineHCID 61229Vanillin acetateHCID 517045Sodium Acetate

생성물 1

HCID 2623485-Bromo-4-formyl-2-methoxyphenyl acetate

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water
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용매

반응 조건

온도
45 °C

실험 절차

To a mixture of 4-acetoxy-3-methoxybenzaldehyde (75.7 g), anhydrous sodium acetate (76 g) and iodine (0.8 g) in acetic acid (300 ml) is added bromine (21 ml). The mixture is warmed to 45° C. for about 1 hour, then stirred stirred at room temperature for 3 days, poured into water (700 ml) and filtered. The solid is dissolved in toluene and the solution washed with brine, dried over magnesium sulfate, filtered and concentrated in vacuo. The residue is recrystallized twice from hexanes to give the desired product.

후처리

  1. stirringstirred at room temperature for 3 days
  2. filtrationfiltered
  3. dissolutionThe solid is dissolved in toluene
  4. washthe solution washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue is recrystallized twice from hexanes

출처 및 근거

ORD 기록
ord-8a80e624349342b3b650619df4c01469
출처 데이터셋
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05571506

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