Lithium Hydroxide → 4-{[1h-Benzimidazol-2-yl(4-tert-butylcyclohexyl)amino]methyl}benzoic acid

HRID 229983ノート

反応式

HRID 229983 の反応式
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]([CH2:21][C:22]1[CH:31]=[CH:30][C:25]([C:26]([O:28]C)=[O:27])=[CH:24][CH:23]=1)[CH:11]1[CH2:16][CH2:15][CH:14]([C:17]([CH3:20])([CH3:19])[CH3:18])[CH2:13][CH2:12]1.[Li+].[OH-]>O1CCOCC1.O>[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]([CH2:21][C:22]1[CH:31]=[CH:30][C:25]([C:26]([OH:28])=[O:27])=[CH:24][CH:23]=1)[CH:11]1[CH2:16][CH2:15][CH:14]([C:17]([CH3:18])([CH3:19])[CH3:20])[CH2:13][CH2:12]1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 68837482Methyl 4-{[1H-benzimidazol-2-yl(4-tert-butylcyclohexyl)amino]methyl}-benzoate

生成物 1

HCID 688356554-{[1h-Benzimidazol-2-yl(4-tert-butylcyclohexyl)amino]methyl}benzoic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
40 °C

実験手順

To the title compound of Example 1 Step C (0.21 mmol, 90 mg) in 2 mL of dioxane was added a solution of LiOH (2.1 mmol, 52 mg) in 0.6 mL of H2O. The reaction was stirred at 40° C. for 3 h. The product was partitioned into EtOAc/H2O acidified with 2 N HCl. The aqueous phase was washed with EtOAc and the combined organic phase was dried with MgSO4 and concentrated under reduced pressure affording a yellow solid. HPLC A: 1.98 min.

後処理

  1. customThe product was partitioned into EtOAc/H2O
  2. washThe aqueous phase was washed with EtOAc
  3. dry with materialthe combined organic phase was dried with MgSO4
  4. concentrationconcentrated under reduced pressure
  5. customaffording a yellow solid
  6. custom1.98 min.

出典と根拠

ORDレコード
ord-053797de5869425bb0b20c5ab2f8b347
出典データセット
uspto-grants-2009_07
特許番号
US07563815B2

反応ノート

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