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Potassium Hydroxide → 5-Cyclopropyl-2-(4-fluorophenyl)-6-((methylsulfonyl)amino)-3-benzofurancarboxylic acid

HRID 2272288
ノート
印刷プレビュー

反応式

HRID 2272288 の反応式
[CH3:1][S:2]([N:5](S(C)(=O)=O)[C:6]1[C:25]([CH:26]2[CH2:28][CH2:27]2)=[CH:24][C:9]2[C:10]([C:20]([O:22]C)=[O:21])=[C:11]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=3)[O:12][C:8]=2[CH:7]=1)(=[O:4])=[O:3].[OH-].[K+]>C(O)C.O>[CH:26]1([C:25]2[C:6]([NH:5][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:7][C:8]3[O:12][C:11]([C:13]4[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=4)=[C:10]([C:20]([OH:22])=[O:21])[C:9]=3[CH:24]=2)[CH2:27][CH2:28]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 2

HCID 14797Potassium HydroxideHCID 67355848Methyl 6-[bis(methylsulfonyl)amino]-5-cyclopropyl-2-(4-fluorophenyl)-1-benzofuran-3-carboxylate

生成物 1

HCID 673529905-Cyclopropyl-2-(4-fluorophenyl)-6-((methylsulfonyl)amino)-3-benzofurancarboxylic acid

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A suspension of methyl 6-[bis(methylsulfonyl)amino]-5-cyclopropyl-2-(4-fluorophenyl)-1-benzofuran-3-carboxylate (2.88 g, 5.98 mmol) in ethanol (50 mL) and water (25 mL) was treated with potassium hydroxide (6.71 g, 120 mmol) and heated at reflux for 1 hour (the suspension went into solution upon heating). The reaction was concentrated under vacuum, water (100 mL) was added and the solution acidified with 2M HCl (50 mL). The resulting precipitate was filtered, washed with 0.5 M HCl, then dissolved in methanol. This solution was evaporated to dryness and azeotroped twice with toluene to give 5-Cyclopropyl-2-(4-fluorophenyl)-6-[(methylsulfonyl)amino]-1-benzofuran-3-carboxylic acid. LCMS (m/z, ES+)=390 (M+H+).

後処理

  1. temperatureheated
  2. temperatureat reflux for 1 hour (the suspension
  3. temperatureupon heating)
  4. concentrationThe reaction was concentrated under vacuum, water (100 mL)
  5. additionwas added
  6. filtrationThe resulting precipitate was filtered
  7. washwashed with 0.5 M HCl
  8. dissolutiondissolved in methanol
  9. customThis solution was evaporated to dryness
  10. customazeotroped twice with toluene

出典と根拠

ORDレコード
ord-223f41fa53b24517baba40a5ff2968c1
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09119868B2

反応ノート

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