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. 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, A new synthetic method of this compound is introduced below., Quality Control of 1-Bromo-2,3-dichlorobenzene
Intermediate 45:[0178] To a -30C solution of l-bromo-2,3-dichlorobenzene (10 g, 44 mmol) in THF (120 mL) was added z-PrMgCl (2.0 M in THF, 35 mL, 70 mmol) at a rate such that the temperature < -20C. Meanwhile, to a -10C solution of Cul (420 mg, 2.2 mmol) in THF (120 mL) was added pyridine (7.1 mL, 88 mmol) and then benzyl carbonochloridate (9.7 mL, 68 mmol) such that the temperature < 0C. To this heterogeneous mixture was added the initially formed Grignard at a rate such that the temperature < 0C. The resulting solution was stirred at 0C for 30 min and then allowed to warm to rt. The reaction was then quenched with 10% aq NH4C1. EtOAc was added and the blue aq layer was removed. The organic layer was washed with 10% aq H4CI, 1 N HC1, and a 20% aq NaCl solution. The organic layer was then concentrated and the residue was dissolved and crystallized from MeOH. The slurry was filtered and the filtercake washed with MeOH to give benzyl 4-(2,3-dichlorophenyl)pyridine-l(4H)- carboxylate (intermediate 45) (12 g, 76%) as an off-white solid. HPLC: 99%, RT 4.118 min. MS (ESI) m/z 382.0 [M + Na]+. mp: 69-70C.
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; THE UNIVERSITY OF NORTH CAROLINA AT CHAPEL HILL; JIN, Jian; ROTH, Bryan; FRYE, Stephen; WO2012/3418; (2012); A2;,
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