4897-68-1, name is 1-Bromo-2-iodo-4-methoxybenzene, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C7H6BrIO
To a flame-dried two-necked flask (100mL) containing a magnetic stirrer, 65 CuI (0.183g, 0.96mmol), 66 dl-pipecolic acid (0.124g, 0.96mmol) and 67 Cs2CO3 (4.18g, 12.80mmol) in 50 68 mLof DMF/69 1,4-dioxane (1/9) was added 70 4-methoxylbenzyl mercaptan (1.07mL, 7.69mmol) and the reaction mixture was stirred at room temperature for 3min 9 4-Bromo-3-iodoanisole (4)(2.0g, 6.41mmol) was then added into the mixture and the resulting solution was heated to 100C and stirred at this temperature for 24h. After cooling to room temperature, the mixture was filtrated through celite and washed with EtOAc (20mL), the organic layer was added saturated 71 aqueous NaCl solution (100mL) and was extracted with EtOAc (50mL×3). The combined organic extracts were dried over anhydrous MgSO4(S). After filtration and removal of solvent, the residue was purified by column chromatography on silica gel using 10/1 (Hexane/EtOAc) as elution to give 11 compound 5 (1.60g, 75%) as a red oil. Rf=0.30 (20:1 Hex/EtOAc); 1H NMR (500MHz, CDCl3) delta 3.72 (s, 3H), 3.79 (s, 3H), 4.10 (s, 2H), 6.58 (dd, J=9.0, 3.0Hz, 1H), 6.78 (d, J=3.0Hz, 1H), 6.85 (d, J=9.0Hz, 2H), 7.29 (d, J=9.0Hz, 2H), 7.41 (d, J=9.0Hz, 1H); 13C{H} NMR (125MHz, CDCl3) delta 37.3, 55.2, 55.4, 112.3, 113.6, 113.9, 114.4, 127.8, 130.0, 133.2, 138.9, 158.9, 159.0; MS (EI, m/z) 340 (M+, 7), 338 (6), 138 (7), 121 (100), 71 (8), 57 (8); HRMS (EI-magnetic sector) m/z: calcd for C15H15BrO2S 339.9956, found 339.9979.
The synthetic route of 4897-68-1 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Wen, Shi-Ming; Lin, Cheng-Han; Chen, Chin-Chau; Wu, Ming-Jung; Tetrahedron; vol. 74; 20; (2018); p. 2493 – 2499;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com