反応 #1095842

反応方程式

DMF

compound 1

3-Iodocarbazole

tributylamine

methyl acrylate

compound 1

3-Iodocarbazole

→

compound 7

収率 62.0%

3-Methoxycarbonylvinylcarbazole

収率 62.0%

溶媒

H2O

反応条件

後処理

1. 1
   その他to react at 160° C. for 10 minutes
2. 2
   その他The palladium powder was removed by Kiriyama filtration
3. 3
   その他the reaction solution was purified by column chromatography (HexH:AcOEt=3:1)

実験手順

To a DMF solution (0.25 mL) of palladium acetate (38.0 mg, 0.17 μmol), compound 1 (0.50 g, 1.71 mmol), tributylamine (0.41 μL, 1.71 mmol), methyl acrylate (0.38 L, 4.27 mmol), and H2O (1.0 mL) were sequentially added. The reaction solution was allowed to react at 160° C. for 10 minutes using microwaves, and the reaction was traced by TLC. Thereby, the loss of compound 1 was confirmed. The palladium powder was removed by Kiriyama filtration, and then the reaction solution was purified by column chromatography (HexH:AcOEt=3:1), and thus compound 7 (0.26 g, 62%) was obtained as a white powder.

出典