반응 #49524

반응 방정식

trifluoroacetic acid

triethylsilane

4-chloro-5-methoxy-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone

water

→

4-chloro-5-methoxy-7-iodoisoindolinone

수율 64.2%

용매

nitromethane

hexane

ethyl acetate

반응 조건

후처리

1. 1
   여과The precipitated solid was collected by filtration
2. 2
   세척washed with hexane and water
3. 3
   기타by drying under reduced pressure

실험 절차

In a similar manner to Step 4 of Example 16, 4-chloro-5-methoxy-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (300 mg, 0.655 mmol) was dissolved in nitromethane (5 mL), and the solution was treated with trifluoroacetic acid (0.505 mL, 6.55 mmol) and triethylsilane (0.212 mL, 1.31 mmol), followed by stirring at room temperature for 24 hours. The reaction mixture was added with water, ethyl acetate and hexane. The precipitated solid was collected by filtration and washed with hexane and water, followed by drying under reduced pressure to obtain 4-chloro-5-methoxy-7-iodoisoindolinone (136 mg, yield 64%).

출처