反応 #62378

反応方程式

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

5-vinyl-benzo[1,3]dioxole

2-(di-tert-butylphosphino)biphenyl

triethylamine

→

title compound

収率 13.8%

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

収率 13.8%

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度After cooling to room temperature
2. 2
   workup.ADDITION5 g of silica gel was added
3. 3
   その他the solvent was evaporated
4. 4
   その他purified by silica gel column chromatography
5. 5
   その他to obtain 468 mg of the crude product as yellow crystal
6. 6
   洗浄This crude product was washed with 50% diethylether solution in hexane
7. 7
   その他the solvent was evaporated

実験手順

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.

出典