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Methanol → 3-[Methyl(methylsulfonyl)amino]-5-(2-oxo-4-phenylpyrrolidin-1-yl)benzoic acid

HRID 1160455
ノート
印刷プレビュー

反応式

HRID 1160455 の反応式
[CH3:1][N:2]([S:25]([CH3:28])(=[O:27])=[O:26])[C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([N:13]2[CH2:17][CH:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:15][C:14]2=[O:24])[CH:12]=1)[C:6]([O:8]C)=[O:7].[OH-].[Na+].CO>O1CCCC1>[CH3:1][N:2]([S:25]([CH3:28])(=[O:27])=[O:26])[C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([N:13]2[CH2:17][CH:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:15][C:14]2=[O:24])[CH:12]=1)[C:6]([OH:8])=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 57815124Methyl 3-[methyl(methylsulfonyl)amino]-5-(2-oxo-4-phenylpyrrolidin-1-yl)benzoate

生成物 1

HCID 578150783-[Methyl(methylsulfonyl)amino]-5-(2-oxo-4-phenylpyrrolidin-1-yl)benzoic acid収率 91%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of methyl 3-[methyl(methylsulfonyl)amino]-5-(2-oxo-4-phenylpyrrolidin-1-yl)benzoate obtained in Reference Example 18 329 mg (0.32 mmol), 2N aqueous sodium hydroxide solution (0.5 mL), methanol (0.5 mL) and tetrahydrofuran (0.5 mL) was stirred at room temperature for 15 hours. The solvent was concentrated and the mixture was adjusted by adding 1N hydrochloric acid to pH=3 and the mixture was extracted with ethyl acetate. After drying of the mixture on magnesium sulfate, the solvent was evaporated to give 113 mg (0.291 mmol) of the title compound (yield: 91%).

後処理

  1. concentrationThe solvent was concentrated
  2. additionby adding 1N hydrochloric acid to pH=3
  3. extractionthe mixture was extracted with ethyl acetate
  4. customAfter drying of the mixture on magnesium sulfate
  5. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-69012cf08795437fbf7b85ad4e78b77e
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07816387B2

反応ノート

読み込み中…

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