Water → 4-Iodo-3-methoxybenzoic acid

HRID 471820노트

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HRID 471820 반응식
[I:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8]C)=[O:7])=[CH:4][C:3]=1[O:12][CH3:13].[OH-].[Na+].O>CO>[I:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[O:12][CH3:13]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 11243290Methyl 4-iodo-3-methoxybenzoate

생성물 1

HCID 179342274-Iodo-3-methoxybenzoic acid

시약·촉매·용매 1

HCID 887Methanol용매

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온도
65 °C

실험 절차

A mixture of methyl 4-iodo-3-(methyloxy)benzoate (3.25 g, 0.011 mol), sodium hydroxide (0.48 g, 0.012 mol) and water (30 mL) in methanol (30 mL) was heated in an oil bath at 65° C. for 3 hr. The mixture was concentrated in vacuo to remove the methanol and the aqueous residue was chilled in an ice bath. Concentrated aqueous hydrogen chloride was added until the pH was acidic and the mixture was stirred at ice bath temperature. The resulting solid was filtered, washed with water and dried to give 4-iodo-3-(methyloxy)benzoic acid as a white solid, used without further purification. LC/MS (method A) tR 2.35 min; m/z 279 (M+H).

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. customto remove the methanol
  3. temperaturethe aqueous residue was chilled in an ice bath
  4. additionConcentrated aqueous hydrogen chloride was added until the pH
  5. filtrationThe resulting solid was filtered
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-7bc9f6b1d6e64a91be4cd3d5b52c5c73
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633175B2

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