Sodium Hydroxide → HCID 58975120、化合物

HRID 1178920ノート

反応式

HRID 1178920 の反応式
[OH-].[Na+].C[O:4][C:5](=[O:27])[C:6]1[CH:11]=[CH:10][C:9]([S:12]([N:15]2[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:17]([CH:24]([CH3:26])[CH3:25])=[CH:16]2)(=[O:14])=[O:13])=[CH:8][CH:7]=1>C1COCC1.C([O-])(O)=O.[Na+]>[CH:24]([C:17]1[C:18]2[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:15]([S:12]([C:9]2[CH:8]=[CH:7][C:6]([C:5]([OH:27])=[O:4])=[CH:11][CH:10]=2)(=[O:13])=[O:14])[CH:16]=1)([CH3:26])[CH3:25]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 58975020HCID 58975020、化合物

生成物 1

HCID 58975120HCID 58975120、化合物収率 89.3%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

Add five molar NaOH (1.5 mL 0.0075 mol) to a stirring solution of 4-(3-isopropyl-indole-1-sulfonyl)-benzoic acid methyl ester (0.230 g, 0.00061 mol) in THF (10.0 mL) at ambient temperature under N2. Stir the resulting mixture overnight Dilute with 5% NaHCO3 (75 mL) and extract with Et2O. Separate the aqueous layer and acidify with 37% HCl. Extract the resulting precipitate into EtOAc, wash with brine, dry (MgSO4), filter and evaporate giving 0.187 g of the title compound as an off white solid: Mass spectrum (m/e) (M−H) 342.0800; Found (M−H) 342.0802.

後処理

  1. extractionextract with Et2O
  2. customSeparate the aqueous layer
  3. extractionExtract the resulting precipitate into EtOAc
  4. washwash with brine
  5. dry with materialdry (MgSO4)
  6. filtrationfilter
  7. customevaporate

出典と根拠

ORDレコード
ord-ac2cdf0f133a433cb2b035591485ddc6
出典データセット
uspto-grants-2007_10
特許番号
US07276516B2

反応ノート

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