Introduction of a new synthetic route about 328-73-4

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-Iodo-3,5-bis(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference of 328-73-4, The chemical industry reduces the impact on the environment during synthesis 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, I believe this compound will play a more active role in future production and life.

To a solution of compound 13a (125 mg, 0.412 mmol), and Et3N (1 mL) in DMF (4 mL), 1-iodo-3,5-bis(trifluoromethyl)benzene (146 muL, 0.824 mmol), CuI (15.7 mg, 0.082 mmol) and Pd(PPh3)4 (47.7 mg, 0.041 mmol) were added. The reaction mixture was stirred at room temperature overnight and filtered through a SiO2 pad. The residue was washed with 50percent EtOAc/hexane (4.x.15 mL) and concentrated in vacuo. The residue was purified by flash chromatography using 10percent EtOAc in hexane to afford 11a (138 mg, 65percent yield) as white solid. Rf (20percent EtOAc in hexane) 0.71; 1H NMR (300 MHz, CDCl3) delta 7.89 (s, 2H), 7.82 (s, 1H), 7.54-7.51 (m, 2H), 7.45-7.40 (m, 2H), 5.57 (s, 1H), 5.39 (br s, 1H), 4.55 (d, J=11.3 Hz, 2H), 4.11 (d, J=11.5 Hz, 2H), 1.50 (s, 9H); 13C NMR (75 MHz, CDCl3) delta 154.3, 137.1, 131.9, 129.4, 128.4, 128.4, 126.0, 124.6, 122.1, 102.0, 88.3, 82.9, 80.5, 72.8, 47.9, 28.4; IR (CH2Cl2): 3702, 3669, 3602, 3426, 2983, 2923, 2869, 1720, 1606, 1491, 1457, 1385, 1372, 1181, 1142; LRMS (EI): m/z 496 ([M+-F], 2), 459 (3), 430 (2), 399 (1); HRMS (EI): m/z calcd for C25H23NO4F5 [M+-F]: 496.1544, found: 496.1547.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-Iodo-3,5-bis(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ko, Rebecca Y. Y.; Chu, John C. K.; Chiu, Pauline; Tetrahedron; vol. 67; 14; (2011); p. 2542 – 2547;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com