تفاعل #62378

معادلة التفاعل

6-fluoro-3-iodo-5-nitro-1-trityl-1H-indazole

5-vinyl-benzo[1,3]dioxole

2-(di-tert-butylphosphino)biphenyl

triethylamine

→

title compound

المردود 13.8%

3-[(E)-2-(Benzo[1,3]dioxol-5-yl)-vinyl]-6-fluoro-5-nitro-1-trityl-1 h-indazole

المردود 13.8%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling to room temperature
2. 2
   workup.ADDITION5 g of silica gel was added
3. 3
   أخرىthe solvent was evaporated
4. 4
   أخرىpurified by silica gel column chromatography
5. 5
   أخرىto obtain 468 mg of the crude product as yellow crystal
6. 6
   غسيلThis crude product was washed with 50% diethylether solution in hexane
7. 7
   أخرىthe solvent was evaporated

الإجراء التجريبي

Under nitrogen atmosphere, 1 g of 6-fluoro-3-iodo-5-nitro-1-trityl-1H-indazole was dissolved in 10 mL of acetonitrile, added successively with 1.35 g of 5-vinyl-benzo[1,3]dioxole, 81.7 mg of palladium acetate (II), 162 mg of 2-(di-tert-butylphosphino)biphenyl and 2 mL of triethylamine, and stirred at 100° C. for 5 hours. After cooling to room temperature, 5 g of silica gel was added, and the solvent was evaporated, and purified by silica gel column chromatography, to obtain 468 mg of the crude product as yellow crystal. This crude product was washed with 50% diethylether solution in hexane, and the solvent was evaporated, to afford 143 mg of the title compound as yellow crystals.

المصدر