Ethyl 2-(4-(3,4-dimethoxybenzyloxy)-3-chlorobenzamido)-5-phenoxybenzoate → 2-(4-(3,4-Dimethoxybenzyloxy)-3-chlorobenzamido)-5-phenoxybenzoic acid

HRID 2099961ノート

反応式

HRID 2099961 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:36]=[CH:37][C:38]=1[O:39][CH3:40])[CH2:6][O:7][C:8]1[CH:34]=[CH:33][C:11]([C:12]([NH:14][C:15]2[CH:25]=[CH:24][C:23]([O:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[CH:22][C:16]=2[C:17]([O:19]CC)=[O:18])=[O:13])=[CH:10][C:9]=1[Cl:35]>C1COCC1.CO.O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:36]=[CH:37][C:38]=1[O:39][CH3:40])[CH2:6][O:7][C:8]1[CH:34]=[CH:33][C:11]([C:12]([NH:14][C:15]2[CH:25]=[CH:24][C:23]([O:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[CH:22][C:16]=2[C:17]([OH:19])=[O:18])=[O:13])=[CH:10][C:9]=1[Cl:35]

参加物

5

反応物 1

HCID 57796889Ethyl 2-(4-(3,4-dimethoxybenzyloxy)-3-chlorobenzamido)-5-phenoxybenzoate

生成物 1

HCID 577968912-(4-(3,4-Dimethoxybenzyloxy)-3-chlorobenzamido)-5-phenoxybenzoic acid

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 1C (160 mg, 0.29 mmol) in THF (30 mL) and MeOH (10 mL) at 0° C. was treated with a solution of LiOH monohydrate (60 mg, 1.42 mmol) in water (10 mL). The resulting solution was stirred for 16 hours, and then concentrated to 10 mL. The resulting suspension was taken up in water (10 mL) and brought to pH 5 with 1 N HCl. The solution was extracted with EtOAc (4×25 mL), dried (Na2SO4), filtered and concentrated to afford the 1D as a white solid. (130 mg, 84%).

後処理

  1. concentrationconcentrated to 10 mL
  2. extractionThe solution was extracted with EtOAc (4×25 mL)
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-ff6af964ef47478a9bf4887ea6f908e9
出典データセット
uspto-grants-2009_08
特許番号
US07569725B2

反応ノート

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