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Lithium Hydroxide → 4-(3-Pyridylmethyloxymethyl)-2-phenylbenzoic acid

HRID 2121158
ノート
印刷プレビュー

反応式

HRID 2121158 の反応式
C[O:2][C:3](=[O:25])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][O:11][CH2:12][C:13]2[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=2)=[CH:6][C:5]=1[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[OH-].[Li+]>CO>[N:15]1[CH:16]=[CH:17][CH:18]=[C:13]([CH2:12][O:11][CH2:10][C:7]2[CH:8]=[CH:9][C:4]([C:3]([OH:25])=[O:2])=[C:5]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH:6]=2)[CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 540573764-(3-Pyridylmethyloxymethyl)-2-phenylbenzoic acid methyl ester

生成物 1

HCID 234361714-(3-Pyridylmethyloxymethyl)-2-phenylbenzoic acid収率 93.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution in methanol (5 mL) of [4-(3-pyridylmethyloxymethyl)-2-phenylbenzoic acid methyl ester (0.58 g), prepared as in Example 183A, was added saturated aqueous lithium hydroxide and the reaction mixture was stirred overnight at ambient temperature. The reaction mixture was warmed to 60° C. and stirred for 4 hours. The reaction mixture was concentrated in vacuo and the residue was taken up in water. The aqueous phase was taken to pH 5 with aqueous 3N HCl and extracted with chloroform. The organic phase was concentrated in vacuo to give 4-(3-pyridylmethyloxymethyl)-2-phenylbenzoic acid (0.52 g).

後処理

  1. temperatureThe reaction mixture was warmed to 60° C.
  2. stirringstirred for 4 hours
  3. concentrationThe reaction mixture was concentrated in vacuo
  4. extractionextracted with chloroform
  5. concentrationThe organic phase was concentrated in vacuo

出典と根拠

ORDレコード
ord-454e01ac0f8141d5a0214d53f659d1c9
出典データセット
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06693123B2

反応ノート

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