Potassium Hydroxide → 2-(2-Cyclobutoxy-3-methyl-benzoylamino)-4,5-dichloro-indan-2-carboxylic acid

HRID 1047874ノート

反応式

HRID 1047874 の反応式
C([O:3][C:4]([C:6]1([NH:17][C:18](=[O:31])[C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([CH3:25])[C:20]=2[O:26][CH:27]2[CH2:30][CH2:29][CH2:28]2)[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[C:11]([Cl:16])[C:12]=2[Cl:15])[CH2:7]1)=[O:5])C.[OH-].[K+]>CCO>[CH:27]1([O:26][C:20]2[C:21]([CH3:25])=[CH:22][CH:23]=[CH:24][C:19]=2[C:18]([NH:17][C:6]2([C:4]([OH:5])=[O:3])[CH2:14][C:13]3[C:8](=[CH:9][CH:10]=[C:11]([Cl:16])[C:12]=3[Cl:15])[CH2:7]2)=[O:31])[CH2:28][CH2:29][CH2:30]1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 685899192-(2-Cyclobutoxy-3-methyl-benzoylamino)-4,5-dichloro-indan-2-carboxylic acid ethyl ester

生成物 1

HCID 251610482-(2-Cyclobutoxy-3-methyl-benzoylamino)-4,5-dichloro-indan-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-(2-Cyclobutoxy-3-methyl-benzoylamino)-4,5-dichloro-indan-2-carboxylic acid ethyl ester (255) (460 mg, 0.99 mmol) is dissolved in EtOH (50 mL) and set to stir at RT. To this solution is added 5M KOH (3 ml). The reaction mixture is stirred at RT overnight. After concentration in vacuo, the residue is dissolved in water (20 mL) and acidified with concentrated HCl to pH 2. The resultant mixture is washed with EtOAc (3×100 ml). Organics are combined and washed with brine, then dried over anhydrous Na2SO4 and concentrated in vacuo. The desired product (256) is obtained as white solid (405 mg, 94%).

後処理

  1. stirringThe reaction mixture is stirred at RT overnight
  2. concentrationAfter concentration in vacuo
  3. dissolutionthe residue is dissolved in water (20 mL)
  4. washThe resultant mixture is washed with EtOAc (3×100 ml)
  5. washwashed with brine
  6. dry with materialdried over anhydrous Na2SO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-cb0d1a9582ca4ac69a72634a47a2d638
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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