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Lithium hydroxide, monohydrate → 2-tert-Butoxy-5-methanesulfonyl-benzoic acid

HRID 1820727
ノート
印刷プレビュー

反応式

HRID 1820727 の反応式
C[O:2][C:3](=[O:19])[C:4]1[CH:9]=[C:8]([S:10]([CH3:13])(=[O:12])=[O:11])[CH:7]=[CH:6][C:5]=1[O:14][C:15]([CH3:18])([CH3:17])[CH3:16].O.[OH-].[Li+]>C1COCC1.O>[C:15]([O:14][C:5]1[CH:6]=[CH:7][C:8]([S:10]([CH3:13])(=[O:12])=[O:11])=[CH:9][C:4]=1[C:3]([OH:19])=[O:2])([CH3:18])([CH3:17])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 586778292-tert-Butoxy-5-methanesulfonyl-benzoic acid methyl ester

生成物 1

HCID 211002592-tert-Butoxy-5-methanesulfonyl-benzoic acid収率 66.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To 2-tert-Butoxy-5-methanesulfonyl-benzoic acid methyl ester (1.58 g) in THF (25 mL) was added a solution lithium hydroxide monohydrate (0.35 g) in water (25 mL), and the reaction mixture was stirred at room temperature for 4 hours. After such time, the THF was removed in vacuo and to the remaining aqueous solution was added 8 mL of 1N HCl solution, leading to precipitation of the compound. The precipitate was filtered off and washed several times with water to yield the title compound (1.00 g) as a white solid. MS (m/e): 289.9 (M+NH4+).

後処理

  1. customAfter such time, the THF was removed in vacuo and to the remaining aqueous solution
  2. additionwas added 8 mL of 1N HCl solution
  3. customleading to precipitation of the compound
  4. filtrationThe precipitate was filtered off
  5. washwashed several times with water

出典と根拠

ORDレコード
ord-9980a2140b864bdda6c14b5ee7f210ad
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07605163B2

反応ノート

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