Related Products of 329944-72-1, These common heterocyclic compound, 329944-72-1, name is 3-Bromo-5-chlorotoluene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Step 1 : To a solution of 3-bromo-5~chlorotoluene (754 mg, 3,67 mmol) in diethyl ether (20 mL) was added dropwise butyllithium (1.5 mL, 3.67 mmol) at -78 C. The resulting solution was stirred at -78 C for 0.5h before addition of 3a (558 mg, 1.835 mmol) as one portion. The reaction mixture was stirred from -78 C to rt over 16h before quenching with sat. NaHC (100 mL), followed by the addition of diethyl ether (50 mL) and ethyl acetate (100 mL). The organic phase was dried over Na2S04, and concentrated on a rotary evaporator. The resulting residue was treated with DMSO (10 mL) to give the solid product 4a, which was collected by filtration, followed by washing with ethyl acetate. The filtrate, after removing the volatiles, was purified on RP-HPLC using 20-100% acetomtrile (0.1%TFA) to give 4a as the TFA salt.
The synthetic route of 329944-72-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; MERCK SHARP & DOHME CORP.; DING, FA-Xiang; JIANG, Jinlong; SHEN, Dong-Ming; SHEN, Hong; SHI, Zhi-Cai; WO2011/137024; (2011); A1;,
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