Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 2265-91-0, name is 1,3-Difluoro-5-iodobenzene, A new synthetic method of this compound is introduced below., Quality Control of 1,3-Difluoro-5-iodobenzene
Example 1.93: Preparation of 2-(((lr,4r)-4-((3-(3,5-Difluorophenyl)-3- phenylureido)methyl)cyclohexyl)methoxy)acetic Acid (Compound 44).; Step A: Preparation of 3,5-Difluoro-iV-phenylaniline.; In a 5 mL microwave reaction vial was placed aniline (0.298 g. 3.20 mmol) and 1,3- difluoro-5-iodobenzene (0.768 g, 3.20 mmol) in toluene (3 mL). KOH (0.323 g, 5.76 mmol) in water (650 muL) and N,N,N-trimethylhexadecan-l-ammium bromide (6.30 mg, 0.017 mmol) were added to the vial with stirring. After the reaction was warmed to 90 0C, bis[tri(f- butylphosphine]palladium[0] (0.016 g, 0.032 mmol) was added and the reaction was stirred at 150 0C for 4 h and then 160 0C for 2 h. The mixture was diluted with water and brine, and extracted with toluene. The toluene extract was subsequently washed with water, dried over MgSO4 and concentrated. The residue was purified by flash column chromatography to provide the title compound as a brown oil (0.132 g). LCMS m/z = 206.2 [M+H]+; 1H nuMR (400 MHz, DMSO-J6) delta ppm 6.54 (tt, J= 9.35, 2.27 Hz, IH), 6.63 (dd, J= 10.48, 2.15 Hz, 2H), 7.01 (dt, 7 = 14.65, 1.14 Hz, IH), 7.17 (dd, J= 8.59, 1.01 Hz, 2H), 7.34 (t, J= 7.83 Hz, 2H), 8.69 (s, IH).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; ARENA PHARMACEUTICALS, INC.; WO2009/117095; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com