反応 #52590

反応方程式

5-chlorosulfonyl-2-oxindole

4-trifluoromethylaniline

pyridine

→

5-(4-trifluoromethylphenyl-aminosulfonyl)-2-oxindole

収率 37.2%

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他The precipitate which formed
2. 2
   ろ過was collected by vacuum filtration
3. 3
   洗浄washed twice with 5 mL of water
4. 4
   その他dried under vacuum at 40° C. overnight
5. 5
   その他to give 2.4 g of crude product
6. 6
   workup.ADDITIONcontaining some impurities by thin layer chromatography
7. 7
   その他The crude product was chromatographed on silica gel eluting with ethyl acetate:hexane (1:2)

実験手順

A suspension of 2.1 g of 5-chlorosulfonyl-2-oxindole, 1.6 g of 4-trifluoromethylaniline and 1.4 g of pyridine in 20 mL of dichloromethane was stirred at room temperature for 4 hours. The precipitate which formed was collected by vacuum filtration, washed twice with 5 mL of water and dried under vacuum at 40° C. overnight to give 2.4 g of crude product containing some impurities by thin layer chromatography. The crude product was chromatographed on silica gel eluting with ethyl acetate:hexane (1:2) to give 1.2 g (37% yield) of 5-(4-trifluoromethylphenyl-aminosulfonyl)-2-oxindole.

出典