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. 620621-48-9, name is Methyl 2-chloro-5-iodobenzoate, A new synthetic method of this compound is introduced below., SDS of cas: 620621-48-9
Intermediate 71 : methyl 2-chloro-5-(4-(dimethylamino)piperidin-l-yl)benzoate; Methyl 2-chloro-5-iodobenzoate (1.0Og, 3.37 mmol), cesium carbonate (0.360 mL,4.50 mmol), BINAP (0.070 g, 0.11 mmol), palladium(II) acetate (0.025 g, 0.11 mmol) and 4-(dimethylamino)piperidine (0.519 g, 4.05 mmol) were suspended in dioxane (18 mL) and sealed into a microwave tube. The reaction was heated to 120 0C for 3 hours in the microwave reactor and cooled to RT. The reaction mixture was filtered through celite. The crude product was purified by flash silica chromatography, elution gradient 0 to 10%NHVMeOH in DCM. Pure fractions were evaporated to dryness to afford methyl 2-chloro- 5-(4-(dimethylamino)piperidin-l-yl)benzoate (0.456 g, 68.3 %) as a yellow oil. m/z (ESI+) (M+H)+ =297.45; HPLC tR = 1.01 min. 1H NMR (400.13 MHz, CDC13) delta 1.56 – 1.66 (2H, m), 1.93 (2H, d), 2.24 – 2.29 (IH, m), 2.31 (6H, s), 2.71 – 2.78 (2H, m), 3.71 (2H, d), 3.92 (3H, s), 6.94 – 6.97 (IH, m), 7.27 – 7.28 (IH, m), 7.33 (IH, d).
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; AstraZeneca AB; AstraZeneca UK Limited; WO2009/47558; (2009); A1;,
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