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Sodium Hydroxide → HCID 57732261、化合物

HRID 401775
ノート
印刷プレビュー

反応式

HRID 401775 の反応式
[Cl:1][C:2]1[S:6][C:5]([NH:7][S:8]([C:11]2[CH:20]=[CH:19][C:14]([C:15]([O:17]C)=[O:16])=[C:13]([F:21])[CH:12]=2)(=[O:10])=[O:9])=[N:4][CH:3]=1.[OH-].[Na+]>O1CCOCC1>[Cl:1][C:2]1[S:6][C:5]([NH:7][S:8]([C:11]2[CH:20]=[CH:19][C:14]([C:15]([OH:17])=[O:16])=[C:13]([F:21])[CH:12]=2)(=[O:10])=[O:9])=[N:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 57731924HCID 57731924、化合物

生成物 1

HCID 57732261HCID 57732261、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Methyl 4-{[(5-chloro-1,3-thiazol-2-yl)amino]sulfonyl}-2-fluorobenzoate (Preparation 32, 3.6 g, 10.26 mmol, 1 eq) was suspended in 2.5M sodium hydroxide (16.5 ml, 41 mmol, 4 eq) and dioxane (4 ml) and the reaction mixture heated at 50° C. for 2 hours. The organic solvent was removed in vacuo and the residue diluted with ethyl acetate (20 ml). The remaining solid was removed by filtration and the organic layer separated. The aqueous phase was acidified with concentrated HCl, extracted into ethyl acetate, washed with brine, dried over magnesium sulphate, filtered and evaporated in vacuo. The title compound was obtained as a white solid (2.74 g, 8.1 mmol, 79%).

後処理

  1. customThe organic solvent was removed in vacuo
  2. additionthe residue diluted with ethyl acetate (20 ml)
  3. customThe remaining solid was removed by filtration
  4. customthe organic layer separated
  5. extractionextracted into ethyl acetate
  6. washwashed with brine
  7. dry with materialdried over magnesium sulphate
  8. filtrationfiltered
  9. customevaporated in vacuo

出典と根拠

ORDレコード
ord-ccad3dbc277b44c8ba4491794beba33e
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08741934B2

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