反应详情

温度

70 °C

To 0.8 g (2.3 mmol) of 3-(4-cyclododecyl-1-oxobutyl)-4-hydroxy-2-(5H)thiophenone in 20 mL of ethanol at 70° C. is added 0.26 g (2.2 mmol) of trishydroxymethyl aminomethane dissolved in 5 mL of water. The reaction mixture is stirred at 70° C. for 0.5 hours and then the solvents are evaporated. The residue is recrystallized from tetrahydrofuran/ether (2:1) to give 0.66 g of an off white solid: m.p. 141°-144° C.; IR (KBr) 3420, 2920, 2830, 1580 cm-1 ; NMR (DMSO-d6) δ1.11.-1.4 (m, 10H), 2.55 (t, J=7 Hz, 2H), 3.26 (s, 1H), 3.31 (s, 4H), 3.47 (d, J=5, 3 Hz), 5.15 (t, J=5 Hz, 2H), 7.6 (bs, 2H); MS (DCI) [M+H]+ 353. Anal. Calc' d. for C4H43NO6S: C 60.86; H 9.15; N, 2.96 Found: C, 60.91; H 9.16; N, 2.88

1. customthe solvents are evaporated
2. customThe residue is recrystallized from tetrahydrofuran/ether (2:1)
3. customto give 0.66 g of an off white solid