Water → 2-(2-Cyclobutoxy-3-methyl-benzoylamino)-indan-2-carboxylic acid

HRID 1047666ノート

反応式

HRID 1047666 の反応式
C([O:3][C:4]([C:6]1([NH:15][C:16](=[O:29])[C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([CH3:23])[C:18]=2[O:24][CH:25]2[CH2:28][CH2:27][CH2:26]2)[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)=[O:5])C.[OH-].[K+].O>CCO>[CH:25]1([O:24][C:18]2[C:19]([CH3:23])=[CH:20][CH:21]=[CH:22][C:17]=2[C:16]([NH:15][C:6]2([C:4]([OH:5])=[O:3])[CH2:7][C:8]3[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=3)[CH2:14]2)=[O:29])[CH2:28][CH2:27][CH2:26]1

参加物

5

反応物 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 593140752-(2-Cyclobutoxy-3-methyl-benzoylamino)-indan-2-carboxylic acid ethyl ester

生成物 1

HCID 251602822-(2-Cyclobutoxy-3-methyl-benzoylamino)-indan-2-carboxylic acid収率 81.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The mixture of 2-(2-cyclobutoxy-3-methyl-benzoylamino)-indan-2-carboxylic acid ethyl ester (8) (250 mg, 0.64 mmol) and KOH (600 mg, 10.7 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 (20 mL) and the solution acidified with conc. HCl until pH˜3 to yield a precipitate. The precipitate is filtered to give a pure product (9) as white solid (190 mg, 81%).

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 (20 mL)
  6. customto yield a precipitate
  7. filtrationThe precipitate is filtered

出典と根拠

ORDレコード
ord-2b2eef3e90e2486caf9f060d096dab49
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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