p-Toluenesulfonic acid monohydrate → HCID 86601087, compound

Participants

Reaction Steps

To a solution of 2,7-bis-(4-methylpiperazin-1-yl)-fluoren-9-one from Example 27A (120 mg, 0.319 mmol) in EtOH-EtOAc (2 mL) was added a solution of p-toluenesulfonic acid monohydrate (60 mg, 0.32 mmol; Aldrich) in EtOH (2 mL). The mixture was stirred overnight and the purple precipitate was collected by filtration to afford the title compound (102 mg, 0.14 mmol; 89% yield based on p-toluenesulfonic acid monohydrate): 1H NMR (300 MHz, CD3OD) δ ppm 7.70 (d, J=8 Hz, 4H), 7.45 (d, J=8 Hz, 2H), 7.19-7.27 (m, 6H), 7.13 (dd, J=8, 2 Hz, 2H), 2.96 (s, 6H), 2.35 (s, 6H); MS (DCl/NH3) m/z 377 (M+H)+; Anal. C23H28N4O.2C7H8O3S.0.1H2O: C, H, N.

Provenance & Evidence