反応 #1537

反応方程式

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

→

pure title compound

収率 72.0%

3-(1-acetoxy-2-chloroethyl)-2-thiophenesulfonamide

収率 72.0%

溶媒

trifluoroacetic acid

反応条件

後処理

1. 1
   濃縮concentrated under reduced pressure
2. 2
   workup.DISSOLUTIONThe residue was dissolved in methylene chloride
3. 3
   洗浄the solution was washed with aqueous sodium bicarbanate solution
4. 4
   その他The organic layer was separated
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   ろ過filtered
7. 7
   濃縮The filtrate was then concentrated

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.

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