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Water → 3-Amino-6-chloro-2-hydroxy-N-methoxy-N-ethyl-benzenesulfonamide

HRID 1024571
ノート
印刷プレビュー

反応式

HRID 1024571 の反応式
[CH2:1]([N:3]([O:21][CH3:22])[S:4]([C:7]1[C:15]2[O:14]C(C(C)(C)C)=[N:12][C:11]=2[CH:10]=[CH:9][C:8]=1[Cl:20])(=[O:6])=[O:5])[CH3:2].S(=O)(=O)(O)O.O>O1CCOCC1>[NH2:12][C:11]1[C:15]([OH:14])=[C:7]([S:4]([N:3]([O:21][CH3:22])[CH2:1][CH3:2])(=[O:6])=[O:5])[C:8]([Cl:20])=[CH:9][CH:10]=1
参加物反応条件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 962WaterHCID 1118Sulfuric AcidHCID 866386352-tert-Butyl-6-chloro-benzooxazole-7-sulfonic acid ethyl-methoxy-amide

生成物 1

HCID 866386363-Amino-6-chloro-2-hydroxy-N-methoxy-N-ethyl-benzenesulfonamide

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

2-tert-Butyl-6-chloro-benzooxazole-7-sulfonic acid ethyl-methoxy-amide (2.7 g, 7.78 mmol) in dioxane (15 ml) was treated with a mixture of concentrated sulphuric acid (3.5 ml) and water (3.5 ml). The reaction mixture was heated at 80° C. for a total of 8 h and then allowed to cool to RT. Dioxane was removed in vacuo and the resulting aqueous mixture was treated with 1M NaOH (aq) until pH7 was attained. The reaction mixture was extracted with EtOAc, dried (MgSO4) and concentrated in vacuo to afford the title compound as a brown solid; [M+H]+ 281.1.

後処理

  1. temperatureto cool to RT
  2. customDioxane was removed in vacuo
  3. additionthe resulting aqueous mixture was treated with 1M NaOH (aq) until pH7
  4. extractionThe reaction mixture was extracted with EtOAc
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9a724d3ff7104b5cbe39a9bd39be7cae
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722925B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート