反応 #1533

反応方程式

N-t-butyl-3-(1-aceoxy-2-fluoroethyl) 2-thiophenesulfonamide

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

→

pure title compound

収率 74.0%

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

収率 74.0%

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washed with aqueous sodium bicarbonate 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 concentrated
8. 8
   その他The residue was recrystallized

実験手順

1.4 g (0.0043 mole) of N-t-butyl-3-(1-aceoxy-2-fluoroethyl) -2-thiophenesulfonamide synthesized in Example 2 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 washed with aqueous sodium bicarbonate solution. The organic layer was separated, dried over anhydrous magnesium sulfate and then filtered. The filtrate was concentrated. The residue was recrystallized to obtain 750 mg (Yield: 74%) of the pure title compound as a white solid.

出典