Citric Acid → 4-(3-chlorophenyl)sulfonylbenzoic acid

HRID 1911147ノート

反応式

HRID 1911147 の反応式
C[O:2][C:3](=[O:20])[C:4]1[CH:9]=[CH:8][C:7]([S:10]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=2)(=[O:12])=[O:11])=[CH:6][CH:5]=1.[Li+].[OH-].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>C1COCC1.CO.O>[Cl:19][C:15]1[CH:14]=[C:13]([S:10]([C:7]2[CH:8]=[CH:9][C:4]([C:3]([OH:20])=[O:2])=[CH:5][CH:6]=2)(=[O:11])=[O:12])[CH:18]=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 311Citric AcidHCID 3939Lithium HydroxideHCID 59625905HCID 59625905、化合物

生成物 1

HCID 3438084-(3-chlorophenyl)sulfonylbenzoic acid

試薬・触媒・溶媒 1

HCID 21892291Methanol tetrahydrofuran water溶媒

実験手順

A mixture of compound 31a (138 mg, 0.44 mmol) and LiOH (42 mg, 1.77 mmol) in THF/MeOH/H2O (2/2/2 mL) was stirred for 4 h. A 15% citric acid solution (10 mL) was added. The mixture was then extracted with EtOAc (3×). The combined organic extracts were washed with brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The resultant residue, compound 31b (130 mg) was dried under reduced pressure for 18 h and used without further purification.

後処理

  1. extractionThe mixture was then extracted with EtOAc (3×)
  2. washThe combined organic extracts were washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. dry with materialThe resultant residue, compound 31b (130 mg) was dried under reduced pressure for 18 h
  7. customused without further purification

出典と根拠

ORDレコード
ord-188be11f64ef42f3876eee02103414f1
出典データセット
uspto-grants-2013_12
特許番号
US08604017B2

反応ノート

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