Citric Acid → HCID 57901602、化合物

HRID 1851490ノート

反応式

HRID 1851490 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[C:10]([NH:12][S:13]([C:16]3[S:17][CH:18]=[CH:19][CH:20]=3)(=[O:15])=[O:14])[CH:11]=1)[NH:8][C:7]([C:21]([O:23]CC)=[O:22])=[CH:6]2.CO.[OH-].[K+].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>O1CCCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[C:10]([NH:12][S:13]([C:16]3[S:17][CH:18]=[CH:19][CH:20]=3)(=[O:15])=[O:14])[CH:11]=1)[NH:8][C:7]([C:21]([OH:23])=[O:22])=[CH:6]2

参加物

6

反応物 4

HCID 311Citric AcidHCID 887MethanolHCID 14797Potassium HydroxideHCID 57901653HCID 57901653、化合物

生成物 1

HCID 57901602HCID 57901602、化合物収率 96%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixed solution of ethyl 5-methoxy-7-[(2-thienylsulfonyl)amino]-1H-indole-2-carboxylate (0.34 g) in tetrahydrofuran (10 mL)-methanol (10 mL) was added aqueous solution (5 mL) of 85% potassium hydroxide (0.20 g), and the mixture was stirred at room temperature for 15 hr. Aqueous citric acid solution was added to the reaction mixture, and the mixture was extracted with ethyl acetate, washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained crystals were washed with ethyl acetate-hexane to give the title compound (300 mg, yield 96%) as pale-yellow crystals. melting point>240° C. (decomposition).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washwashed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. washThe obtained crystals were washed with ethyl acetate-hexane

出典と根拠

ORDレコード
ord-029eeebeb4e3404cb3a5025de3d214d9
出典データセット
uspto-grants-2015_02
特許番号
US08957070B2

反応ノート

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