Related Products of 103962-05-6, These common heterocyclic compound, 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Resin 3 (120 mg, 0.084 mmol) was swelled in DCM (2 mL) for 1 h and drained. A solution of 4-(trifluoromethoxy)iodobenzene 4 (96.8 mg, 0.336 mmol) and Et3N (150 mL, 1.10 mmol) in DMF (2.0 mL) was purged with a streamof N2 bubbles for two minutes and added to the resin. After mixing for 5 min, PdCl2(PPh3)2 (18.0 mg, 0.025 mmol) andCuI (8.0 mg, 0.042 mmol) were added and the mixture shaken for 24 h. The resin was drained, washed with DMF (3 32 mL), DCM (3 3 2 mL) and cleaved with 10percent TFA/DCM (2.0 mL) for 20 min. The solution was collected and the resinwas rinsed with additional 10percent TFA/DCM (10 mL). The cleavage fractions were combined, treated with neat TFA (3.0mL), stirred for 1 h at rt and concentrated by rotary evaporation to give a crude brown residue. Purification by RP-HPLC(C18 column, CH3CN gradient 5-55percent, 0.1percent TFA, UV analysis 300 nm, 28 min) and lyophilization of the collected fractionsafforded 9.0 mg (25percent yield) of (1S)-N-(2-amino-1-hydroxycarbamoyl-ethyl)-4-(4-trifluoromethoxy-phenylethynyl)-benzamideas a white solid. LRMS (ES+) m/z 408.0 (C19H16F3N3O4 + H requires 408.11); RP-HPLC (300 nm, 28 min run)18.0 min.
The synthetic route of 103962-05-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; The University of Washington; Novartis Vaccines and Diagnostics, Inc.; Andersen, Niels H.; Bowman, Jason; Erwin, Alice; Harwood, Eric; Kline, Toni; Mdluli, Khisimuzi; Ng, Simon; Pfister, Keith B.; Shawar, Ribhi; Wagman, Allan; Yabannavar, Asha; EP2295402; (2015); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com