Carbon Tetrachloride → HCID 11994257, compound

Participants

Reaction Steps

The method follows that of CAQ39 using HAQ105 (60 mg, 0.109 mmol), Ph3P (171.5 mg, 0.654 mmol), CCl4 (190 μL, 1.96 mmol) and dry CH2Cl2 (5 mL). The reaction was stopped after 5 hours of reflux. The product (CAQ190M) was afforded as a dark blue powder (49.8 mg, 78%). M.p. decompose>300° C.; δH (250 MHz; DMSO); 1.5-1.65 (m, 4H, 4×ring-H), 1.75-2.15 (m, 10H, 10×ring-H), 3.4-3.8 (m, 8H, 2×HNCH2CH2N and 4×ring-H), 4-4.1 (q, 4H, 2×HNCH2CH2N), 4.15 (2×d, 4H, 2×NCHCH2Cl) 7.2 (s, 2H, C(2)H and C(3)H), 7.65 (s, 2H, C(6)H and C(7)H), 10.45 (t, 2H, C(1)NH and C(4)NH), and 13.45 (s, 2H, C(5)OH, C(8)OH); δC (62.9 MHz; DMSO), 26.11, 37.05, 42.78, 50.78, 51.83, 60.32, 62.26, 108.41, 114.33, 125.00, 126.56, 145.93, 154.69, 184.28; FAB MS, m/z(M+H)+589.

Provenance & Evidence