反应详情

温度

110 °C

A 10 mL heavy wall vial was charged with trans-cyclohexane diamine (11.8 mg, 0.10 mmol, 0.5 equiv), 3-bromo-5-(3,3-dimethyl-but-1-ynyl)-thiophene-2-carboxylic acid methyl ester (125 mg, 0.41 mmol, 2.0 equiv), K2CO3 (57 mg, 0.41 mmol, 2.0 equiv), CuI (19.7 mg, 0.10 mmol, 0.5 equiv), 5-cyclohexyl-2-(3-hydroxy-propyl)-morpholin-3-one (50 mg, 0.21 mmol, 1.0 equiv) and 1,4-dioxane (0.5 mL). The mixture was flushed with N2 and stirred at 110° C. for 24 hours. The mixture was filtered through celite and the filtrate was concentrated under vacuum. The residue was purified by silica gel, EtOAc/heptane 30% to give product 10 mg (yield 10%).

1. customThe mixture was flushed with N2
2. filtrationThe mixture was filtered through celite
3. concentrationthe filtrate was concentrated under vacuum
4. customThe residue was purified by silica gel, EtOAc/heptane 30%