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Water → 2-(Methylthio)-6-phenylbenzenesulfonamide

HRID 246993
ノート
印刷プレビュー

反応式

HRID 246993 の反応式
O.CC([NH:6][S:7]([C:10]1[C:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:14][CH:13]=[CH:12][C:11]=1[S:22][CH3:23])(=[O:9])=[O:8])(C)C>FC(F)(F)C(O)=O>[CH3:23][S:22][C:11]1[CH:12]=[CH:13][CH:14]=[C:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:10]=1[S:7]([NH2:6])(=[O:9])=[O:8]
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 962WaterHCID 13670365N-(1,1-dimethylethyl)-2-(methylthio)-6-phenylbenzenesulfonamide

生成物 1

HCID 136703672-(Methylthio)-6-phenylbenzenesulfonamide収率 77.6%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

In a mixture of 75 ml trifluoroacetic acid plus 2 ml water was dissolved 10 g (0.030 mol) of N-(1,1-dimethylethyl)-2-(methylthio)-6-phenylbenzenesulfonamide and heated to 85°. After 15 minutes the mixture was cooled and evaporated, then diluted with water and extracted with methylene chloride. The methylene chloride was washed with saturated sodium bicarbonate solution, dried (MgSO4), evaporated in vacuo and crystallized from ether/hexanes to afford 6.5 g of the title compound, m.p. 167°-168°.

後処理

  1. temperatureheated to 85°
  2. temperatureAfter 15 minutes the mixture was cooled
  3. customevaporated
  4. additiondiluted with water
  5. extractionextracted with methylene chloride
  6. washThe methylene chloride was washed with saturated sodium bicarbonate solution
  7. dry with materialdried (MgSO4)
  8. customevaporated in vacuo
  9. customcrystallized from ether/hexanes

出典と根拠

ORDレコード
ord-40a214c9f3e5441fadd260564a5f211c
出典データセット
uspto-grants-1987_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04705556

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