反应详情

温度

80 °C

A solution of 3-[3-[4-(5-methoxy-4-pyrimidyl)-1-piperazinyl]propyl]-5-aminoindole (6) (0.208 g, 0.56 mmol) and 3,4-bis (1-methylethoxy) cyclobut-3-ene-1,2-dione4 (2) (0.112 g, 0.56 mmol) in 5 mL of absolute ethanol was stirred at room temperature for 66 h and then it was heated at ca. 80° C. (oil-bath temperature) for 4 h. The cooled mixture was filtered and the residue was washed with ethanol and then dried in vacuo to give the title compound (0.190 g, 64%) as a slightly pinkish solid, mp 140°-143° C.: IR (KBr) 3312, 1800, 1720, 1607, 1588 cm-1 ; 1H NMR (DMSO-d6, 200 MHz) δ 10.80 (s, 1H), 10.7 (br s, 1H), 8.22 (s, 1H), 8.01 (s, 1H), 7.48 (m, 1H), 7.28 (d, J=8.6 Hz, 1H), 7.14 (s, 1H), 7.06 (m, 1H), 5.40 (m, 1H), 3.81 (s, 3H), 3.65 (br s, 4H), 3.42 (q, J=7.0 Hz, 0.6H, CH3CH2OH), 2.67 (m, 2H), 2.43 (m, 4H), 2.35 (m, 2H), 1.82 (m, 2H), 1.41 (d, J=6.1 Hz, 6H), 1.04 (t, J=7.0 Hz, 0.9H, CH3CH2OH). Anal. Calcd for C27H32N6O4. 0.5 H2O. 0.3 C2H6O: C, 62.85; H, 6.65; N, 15.94. Found: C, 62.85; H, 6.46; N, 16.17.

1. filtrationThe cooled mixture was filtered
2. washthe residue was washed with ethanol
3. customdried in vacuo