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Tetrahydrofuran → 4-{[2-Ethyl-1-(3-methyl-1-benzothiophen-2-yl)butyl]amino}benzoic acid

HRID 2091282
ノート
印刷プレビュー

反応式

HRID 2091282 の反応式
[CH2:1]([CH:3]([CH2:26][CH3:27])[CH:4]([NH:15][C:16]1[CH:25]=[CH:24][C:19]([C:20]([O:22]C)=[O:21])=[CH:18][CH:17]=1)[C:5]1[S:6][C:7]2[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=2[C:9]=1[CH3:10])[CH3:2].O1CCCC1.[OH-].[Na+]>C(O)C>[CH2:26]([CH:3]([CH2:1][CH3:2])[CH:4]([NH:15][C:16]1[CH:17]=[CH:18][C:19]([C:20]([OH:22])=[O:21])=[CH:24][CH:25]=1)[C:5]1[S:6][C:7]2[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=2[C:9]=1[CH3:10])[CH3:27]
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 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 66777962Methyl 4-{[2-ethyl-1-(3-methyl-1-benzothiophen-2-yl)butyl]amino}benzoate

生成物 1

HCID 667776494-{[2-Ethyl-1-(3-methyl-1-benzothiophen-2-yl)butyl]amino}benzoic acid収率 95%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a mixture of methyl 4-{[2-ethyl-1-(3-methyl-1-benzothiophen-2-yl)butyl]amino}benzoate (580 mg) synthesized above, tetrahydrofuran (10 mL) and ethanol (10 mL) was added 1N aqueous sodium hydroxide solution (10.0 mL), and the mixture was stirred overnight with heating under reflux, and concentrated under reduced pressure. The residue was dissolved in water (20 mL), and 1N hydrochloric acid (10.0 mL) was added at 0° C. The resulting precipitate was collected by filtration to give the title object compound (529 mg, 95%) as a white solid.

後処理

  1. temperaturewith heating
  2. temperatureunder reflux
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe residue was dissolved in water (20 mL)
  5. addition1N hydrochloric acid (10.0 mL) was added at 0° C
  6. filtrationThe resulting precipitate was collected by filtration

出典と根拠

ORDレコード
ord-fef15a57e4b14fb1a0251f23f02d1ee8
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436043B2

反応ノート

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