Benzoyl chloride, 3-chloro- → HCID 178519571, compound

Participants

Reaction Steps

Synthesized from compound 26. To a solution of compound 26 (0.2 g, 0.6 mmol) in 5 mL of CH2Cl2 was added 1 mmol of TEA and 0.8 mmol of 3-chloro-benzoyl chloride. The reaction was stirred overnight at room temperature. After the solvents were evaporated, the residue was purified with semi-preparative HPLC to afford a solid (16% yield). MP: 147-149° C.; MS (ES−): 436; 1H NMR (400 MHz, CDCl3): 1.88-2.08 (m, 2H), 2.86-3.07 (m, 4H), 3.52-3.71 (m, 4H), 3.81-3.89 (m, 2H), 7.33-7.43 (m, 4H), 7.62 (d, 1H), 7.81 (t, 1H), 7.90 (t, 1H). Anal. Calcd. for C22H21ClN6O2.0.7H2O: C, 54.89; H, 4.39; N, 16.70. Found: C, 54.93; H, 4.43; N, 16.34.

Provenance & Evidence