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Sodium Iodide → 3-Hydroxy-4-iodobenzoic acid

HRID 390623
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HRID 390623 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-].[Na+]>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]
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참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 74203-Hydroxybenzoic AcidHCID 14798Sodium HydroxideHCID 23665760Sodium Hypochlorite

생성물 1

HCID 7368543-Hydroxy-4-iodobenzoic acid수율 31.8%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

21 g (520 mmol) of sodium hydroxide and then 78.7 g (520 mmol) of sodium iodide are added to a solution of 69 g (500 mmol) of 3-hydroxybenzoic acid in 700 mL of methanol. The reaction mixture is cooled to 0° C. and aqueous sodium hypochlorite solution is then added (520 mmol). 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. 41.92 g of 3-hydroxy-4-iodobenzoic acid are obtained in the form of an off-white solid. The aqueous phase is extracted with ethyl acetate, dried over magnesium sulfate, filtered and evaporated and the residue obtained is taken up in heptane and then filtered.

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-e3f504ac44c9462b9c0bd6996b66d575
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08383652B2

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