反应详情

2-Cyclohexyl-8-ethenesulfonyl-1,3,8-triaza-spiro[4.5]dec-1-en-4-one (60.0 mg, 0.184 mmol), 5-bromo-indole (72.0 mg, 0.367 mmol), palladium(II) acetate (4.1 mg, 0.0183 mmol), tris(o-tolyl)phosphine (11.2 mg, 0.0368 mmol), triethylamine (0.077 ml, 0.552 mmol) and DMA (0.6 ml) were mixed in a sealed test tube in an N2 atmosphere. This mixture was irradiated with microwaves (190° C., 20 min). The reaction mixture was cooled, and then quenched with saturated brine and extracted with ethyl acetate three times. The organic layers were combined, sequentially washed with water and saturated brine and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (CH2Cl2-MeOH) to give 2-cyclohexyl-8-[(E)-2-(1H-indol-5-yl)-ethenesulfonyl]-1,3,8-triaza-spiro[4.5]dec-1-en-4-one as a yellow form (40.6 mg, 50%).

1. customThis mixture was irradiated with microwaves (190° C., 20 min)
2. temperatureThe reaction mixture was cooled
3. customquenched with saturated brine
4. extractionextracted with ethyl acetate three times
5. washsequentially washed with water and saturated brine
6. concentrationconcentrated under reduced pressure
7. customThe resulting residue was purified by silica gel column chromatography (CH2Cl2-MeOH)