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

HRID 1441
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HRID 1441 반응식
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]
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참가 물질

3

반응물 1

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

생성물 1

HCID 196907793-(1-Acetoxy-2-chloroethyl)-2-thiophenesulfonamide수율 72%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8f3db3635526422b993dd23dd01d5b7e
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05726127

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