Oxalyl chloride → HCID 71625155, compound

Participants

Reaction Steps

Following the method used to prepare 24a, the use of 1b (0.51 g, 1.60 mmol) and oxalyl chloride (0.32 mL, 3.65 mmol) followed by allowing the intermediate acid chloride to react with MeOH (5 mL) provided 0.95 g (90%) of product 7 as a white solid, mp 230-233° C. 1H NMR (300 MHz, DMSO-d6) δ 2.34 (s, 3H), 3.84 (s, 3H), 7.05 (d, J=8 Hz, 2H), 7.16-7.20 (m, 1H), 7.25-7.28 (m, 3H), 7.45 (d, J=8 Hz, 1H), 12.41 (s, 1H). LC-MS (CI): m/z 332.1 [(M+H)+ C17H14ClNO2S requires 331.04]. Purity (100%). Calcd for C17H14ClNO2S.0.2H2O: C, 60.87; H, 4.33; N, 4.18; S, 9.56; Cl, 10.57. Found: C, 60.89; H, 4.08; N, 4.14; S, 9.81; Cl, 10.77.

Provenance & Evidence