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Hydrochloric Acid → 3-(4-Tert-butylphenylsulfonamido)benzo[b]thiophene-2-carboxylic acid

HRID 1925725
ノート
印刷プレビュー

反応式

HRID 1925725 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH:14][C:15]2[C:16]3[CH:27]=[CH:26][CH:25]=[CH:24][C:17]=3[S:18][C:19]=2[C:20]([O:22]C)=[O:21])(=[O:13])=[O:12])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+].C(#N)C.Cl>CO>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH:14][C:15]2[C:16]3[CH:27]=[CH:26][CH:25]=[CH:24][C:17]=3[S:18][C:19]=2[C:20]([OH:22])=[O:21])(=[O:13])=[O:12])=[CH:7][CH:6]=1)([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6342AcetonitrileHCID 14798Sodium HydroxideHCID 59180462Methyl 3-(4-tert-butylphenylsulfonamido)benzo[b]thiophene-2-carboxylate

生成物 1

HCID 251833683-(4-Tert-butylphenylsulfonamido)benzo[b]thiophene-2-carboxylic acid収率 100.2%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

To a solution of 88 (0.120 g; 0.31 mmol) in methanol (2 mL) was added aqueous sodium hydroxide (1 mL; 2 mmol; 2N). Acetonitrile (2 mL) was added to aid in solubility, and the resulting mixture was stirred overnight. The reaction mixture was acidified with aqueous hydrochloric acid (2N) and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, decanted, and concentrated under reduced pressure. Trituration of the crude product from hexanes and dichloromethane yielded the desired product as a pink solid (121 mg).

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customdecanted
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f937317daac84360b39bd69372390b0e
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08178699B2

反応ノート

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