Dichloromethane → HCID 54767383, compound

Participants

Reaction Steps

2-Hydroxypyridine-1-oxide (0.21 g, 1.9 mmol) was reacted with 4-(chlorosulfonyl)benzoic acid (0.62 g, 2.8 mmol) in 5 mL pyridine. The solvent was evaporated, leaving a yellow oil. Addition of 5 mL of dichloromethane followed by the addition of 5 mL of ethyl acetate allowed for precipitation of PZBG-1e in 30% yield (0.17 g, 0.57 mmol). 1H NMR (400 MHz, DMSO) δ=8.18 (d, J=8.8 Hz, 2H), 8.08 (d, J=8.4 Hz), 7.88 (dd, J1=7.6 Hz, J2=2 Hz), 7.45 (td, J1=8.2 Hz, J2=2 Hz, 1H), 6.50 (dd, J1=9.2 Hz, J2=1.6 Hz, 1H), 6.26 (td, J1=7 Hz, J2=1.6 Hz, 1H). 13C NMR (100 MHz, CDCl3) δ=166.5, 156.6, 141.5, 138.2, 137.9, 137.3, 131.2, 130.4, 122.8, 106.2. ESI-MS(−): m/z 294.26[M−H]−. Anal. calcd. for C12H9NO6S: C, 48.81; H, 3.07; N, 4.74. Found: C, 48.91; H, 3.37; N, 4.84.

Provenance & Evidence