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Methanol → HCID 66726052、化合物

HRID 1042141
ノート
印刷プレビュー

反応式

HRID 1042141 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([O:16][C:17]2[CH:18]=[N:19][C:20]([S:23]([CH3:26])(=[O:25])=[O:24])=[CH:21][CH:22]=2)[CH:5]=[C:6]2[C:10]=1[NH:9][C:8]([C:11]([O:13]CC)=[O:12])=[CH:7]2.CO.[OH-].[K+]>O1CCCC1>[CH3:1][C:2]1[CH:3]=[C:4]([O:16][C:17]2[CH:18]=[N:19][C:20]([S:23]([CH3:26])(=[O:25])=[O:24])=[CH:21][CH:22]=2)[CH:5]=[C:6]2[C:10]=1[NH:9][C:8]([C:11]([OH:13])=[O:12])=[CH:7]2
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 887MethanolHCID 14797Potassium HydroxideHCID 66726116HCID 66726116、化合物

生成物 1

HCID 66726052HCID 66726052、化合物収率 92%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of ethyl 7-methyl-5-{[6-(methylsulfonyl)pyridin-3-yl]oxy}-1H-indole-2-carboxylate (3.9 g), methanol (30 mL), and tetrahydrofuran (50 mL) was added aqueous solution (20 mL) of potassium hydroxide (2.0 g), and the mixture was stirred at room temperature for 15 hr. The reaction solution was concentrated, acidified with aqueous citric acid solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The obtained pale-yellow crystals were washed with ethyl acetate-hexane to give the title compound (3.30 g, yield 92%) as pale-yellow crystals.

後処理

  1. concentrationThe reaction solution was concentrated
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. washThe obtained pale-yellow crystals were washed with ethyl acetate-hexane

出典と根拠

ORDレコード
ord-b32b27ac7d3246c0951df7796460eebc
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08557805B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート