Water → 5-Fluoro-2-(2-isopropoxy-3-methyl-benzoylamino)-indan-2-carboxylic acid

HRID 1047750ノート

反応式

HRID 1047750 の反応式
C([O:3][C:4]([C:6]1([NH:16][C:17](=[O:29])[C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[C:19]=2[O:25][CH:26]([CH3:28])[CH3:27])[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[C:11]([F:15])[CH:12]=2)[CH2:7]1)=[O:5])C.[OH-].[K+].O>CCO>[F:15][C:11]1[CH:12]=[C:13]2[C:8](=[CH:9][CH:10]=1)[CH2:7][C:6]([NH:16][C:17](=[O:29])[C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[C:19]=1[O:25][CH:26]([CH3:27])[CH3:28])([C:4]([OH:5])=[O:3])[CH2:14]2

参加物

5

反応物 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 593144025-Fluoro-2-(2-isopropoxy-3-methyl-benzoylamino)-indan-2-carboxylic acid ethyl ester

生成物 1

HCID 251605405-Fluoro-2-(2-isopropoxy-3-methyl-benzoylamino)-indan-2-carboxylic acid収率 91.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The mixture of 5-fluoro-2-(2-isopropoxy-3-methyl-benzoylamino)-indan-2-carboxylic acid ethyl ester (96) (544 mg, 1.36 mmol) and KOH (1 g, 18 mmol) is dissolved in EtOH (8 mL) and water (1 mL) under a water bath. The water bath is removed when KOH is completely dissolved and the resulting reaction solution is stirred at RT for 8 h. After concentration in vacuo, the residue is dissolved in water (30 mL) and acidified with conc. HCl until no more white precipitate formed. The precipitate is filtered to give a pure product (97) as white solid (460 mg, 91%).

後処理

  1. customThe water bath is removed when KOH
  2. dissolutionis completely dissolved
  3. customthe resulting reaction solution
  4. concentrationAfter concentration in vacuo
  5. dissolutionthe residue is dissolved in water (30 mL)
  6. customformed
  7. filtrationThe precipitate is filtered

出典と根拠

ORDレコード
ord-3a9055b1ba5a4610b490db974017baa4
出典データセット
uspto-grants-2013_10
特許番号
US08569535B2

反応ノート

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