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Hydrochloric Acid → [3-(3-Benzenesulfonylthiophen-2-ylmethyl)-5-chloro-2-methylindol-1-yl]acetic acid

HRID 1944455
ノート
印刷プレビュー

反応式

HRID 1944455 の反応式
C[O:2][C:3](=[O:31])[CH2:4][N:5]1[C:13]2[C:8](=[CH:9][C:10]([Cl:14])=[CH:11][CH:12]=2)[C:7]([CH2:15][C:16]2[S:17][CH:18]=[CH:19][C:20]=2[S:21]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)(=[O:23])=[O:22])=[C:6]1[CH3:30].[OH-].[Li+].Cl>O1CCCC1>[C:24]1([S:21]([C:20]2[CH:19]=[CH:18][S:17][C:16]=2[CH2:15][C:7]2[C:8]3[C:13](=[CH:12][CH:11]=[C:10]([Cl:14])[CH:9]=3)[N:5]([CH2:4][C:3]([OH:31])=[O:2])[C:6]=2[CH3:30])(=[O:23])=[O:22])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1
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 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 67044072[3-(3-Benzenesulfonylthiophen-2-ylmethyl)-5-chloro-2-methylindol-1-yl]acetic acid methyl ester

生成物 1

HCID 58201246[3-(3-Benzenesulfonylthiophen-2-ylmethyl)-5-chloro-2-methylindol-1-yl]acetic acid収率 85.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒

実験手順

A mixture of [3-(3-benzenesulfonylthiophen-2-ylmethyl)-5-chloro-2-methylindol-1-yl]acetic acid methyl ester (0.47 g), 1.0 M aqueous lithium hydroxide solution (2.0 mL) and tetrahydrofuran (2.0 mL) was stirred at room temperature for 1 hour. The mixture was acidified with 1.0 M aqueous hydrochloric acid solution and extracted with ethyl acetate. The combined organic extract was dried using a phase separation cartridge and concentrated under reduced pressure. The residue was purified by crystallisation from a mixture of pentane and ethyl acetate to afford the title compound as a white powder (0.39 g).

後処理

  1. extractionextracted with ethyl acetate
  2. extractionThe combined organic extract
  3. customwas dried
  4. customa phase separation cartridge
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by crystallisation from a mixture of pentane and ethyl acetate

出典と根拠

ORDレコード
ord-6a1c46e5090848c18265bf3d18dd3f96
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08394836B2

反応ノート

読み込み中…

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