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

HRID 1373106ノート

反応式

HRID 1373106 の反応式
[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]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 21074200Methyl 3-methoxy-5-(methylsulfonyl)benzoate

生成物 1

HCID 210741983-Methoxy-5-methylsulfonylbenzoic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-b18111341b304f2986d01d0d1a4d4a4f
出典データセット
uspto-grants-2007_01
特許番号
US07160905B2

反応ノート

読み込み中…