Sodium Iodide → 3-Hydroxy-4-iodobenzoic acid

HRID 250915

반응식

HRID 250915 반응식
[OH-].[Na+].[I-:3].[Na+].[OH:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][CH:14]=1)[C:9]([OH:11])=[O:10].Cl[O-].[K+]>CO>[OH:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[I:3])[C:9]([OH:11])=[O:10]

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 74203-Hydroxybenzoic AcidHCID 14798Sodium HydroxideHCID 23665762Potassium hypochlorite

생성물 1

HCID 7368543-Hydroxy-4-iodobenzoic acid수율 92%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
0 °C

실험 절차

21.0 g (0.52 mol, 1.05 eq) of sodium hydroxide and then 78.7 g (0.52 mol, 1.05 eq) of sodium iodide are added to a solution of 69.1 g (0.5 mol, 1 eq) of 3-hydroxybenzoic acid in 700 ml of methanol. The reaction mixture is cooled to 0° C. and potassium hypochlorite solution (0.52 mol, 1.05 eq) is then added dropwise. The reaction medium is stirred at 0-5° C. for 2 hours and then at room temperature overnight. The methanol is evaporated off and the reaction medium is then acidified with concentrated hydrochloric acid solution. The precipitated product is filtered off, washed with water and dried. 121 g of 3-hydroxy-4-iodobenzoic acid are obtained in the form of an off-white solid. Yield=92%

후처리

  1. customat room temperature
  2. customovernight
  3. customThe methanol is evaporated off
  4. filtrationThe precipitated product is filtered off
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-8659b4409d0a4f239d22195facf37b3e
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863332B2

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