تفاعل #49524

معادلة التفاعل

trifluoroacetic acid

triethylsilane

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

water

→

4-chloro-5-methoxy-7-iodoisoindolinone

المردود 64.2%

المذيبات

nitromethane

hexane

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   ترشيحThe precipitated solid was collected by filtration
2. 2
   غسيلwashed with hexane and water
3. 3
   أخرىby drying under reduced pressure

الإجراء التجريبي

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%).

المصدر