Sodium Thiosulfate → HCID 17747370, compound

Participants

Reaction Steps

A solution of the crude product I2 in DCM was treated with Dess-Martin Periodinane (3.0 eq.) and stirred for 3 h at RT. Aq. sodium thiosulfate was added and the aqueous phase was extracted with DCM. The combined organic phase was dried (Na2SO4) and solvents were removed under reduced pressure. The crude was purified by RP-HPLC (Waters SYMMETRY C18, 7 micron, 19×300 mm; flow: 20 mL/min; Gradient: A: H2O (+0.1% TFA); B: MeCN (+0.1% TFA); 60% A linear to 10% A in 14 min) to afford the title compound as a solid after freeze drying the desired fractions. 1H NMR (300 MHz, DMSO-d6, 300K) δ 7.69-7.50 (3H, m), 8.27-7.92 (4H, m), 8.55 (1H, s). MS (ES+) C15H8F3NOS requires: 307, found: 308 (M+H)+ and 326 (M+H+H20)+.

Provenance & Evidence