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N-t-butyl-3-(1-acetoxy-2-chloroethyl)-2-thiophenesulfonamide → 3-(1-Acetoxy-2-chloroethyl)-2-thiophenesulfonamide

HRID 1441
ノート
印刷プレビュー

反応式

HRID 1441 の反応式
C([NH:5][S:6]([C:9]1[S:10][CH:11]=[CH:12][C:13]=1[CH:14]([O:17][C:18](=[O:20])[CH3:19])[CH2:15][Cl:16])(=[O:8])=[O:7])(C)(C)C>FC(F)(F)C(O)=O>[C:18]([O:17][CH:14]([C:13]1[CH:12]=[CH:11][S:10][C:9]=1[S:6]([NH2:5])(=[O:7])=[O:8])[CH2:15][Cl:16])(=[O:20])[CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 19690764N-t-butyl-3-(1-acetoxy-2-chloroethyl)-2-thiophenesulfonamide

生成物 1

HCID 196907793-(1-Acetoxy-2-chloroethyl)-2-thiophenesulfonamide収率 72%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

1.5 g (0.0044 mole) of N-t-butyl-3-(1-acetoxy-2-chloroethyl)-2-thiophenesulfonamide synthesized in Example 7 was dissolved in 5 ml of trifluoroacetic acid. The reaction solution was stirred at normal temperature for 12 hours and then concentrated under reduced pressure. The residue was dissolved in methylene chloride and the solution was washed with aqueous sodium bicarbanate solution. The organic layer was separated, dried over anhydrous magnesium sulfate and filtered. The filtrate was then concentrated. The residue was subjected to column chromatograpy on silica gel to obtain 760 mg (Yield: 72%) of the pure title compound.

後処理

  1. concentrationconcentrated under reduced pressure
  2. dissolutionThe residue was dissolved in methylene chloride
  3. washthe solution was washed with aqueous sodium bicarbanate solution
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was then concentrated

出典と根拠

ORDレコード
ord-8f3db3635526422b993dd23dd01d5b7e
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05726127

反応ノート

読み込み中…

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