Lithium hydroxide, monohydrate → 3-Methoxy-5-methylsulfonylbenzoic acid

HRID 1373106노트

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HRID 1373106 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([S:13]([CH3:16])(=[O:15])=[O:14])[CH:12]=1)[C:6]([O:8]C)=[O:7].O.[OH-].[Li+]>O1CCOCC1.O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([S:13]([CH3:16])(=[O:15])=[O:14])[CH:12]=1)[C:6]([OH:8])=[O:7]

참가 물질

5

실험 절차

Methyl 3-methoxy-5-methylsulfonylbenzoate (D14) (2.94 g) was dissolved in dioxan (18 ml) and lithium hydroxide monohydrate (0.762 g) in water (18 ml) was added. The mixture was stirred at room temperature for 2 h and then sufficient Amberlyst-15 H+ resin was added to adjust the pH to ˜4. The resin was removed by filtration and washed well with dioxan and the combined filtrates were evaporated. The residue was triturated with ether to give D15 as a pale buff solid (2 crops, 2.29 g).

후처리

  1. additionsufficient Amberlyst-15 H+ resin was added
  2. customThe resin was removed by filtration
  3. washwashed well with dioxan
  4. customthe combined filtrates were evaporated
  5. customThe residue was triturated with ether
  6. customto give D15 as a pale buff solid (2 crops, 2.29 g)

출처 및 근거

ORD 기록
ord-b18111341b304f2986d01d0d1a4d4a4f
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07160905B2

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