Continuously updated synthesis method about C7H6BrCl

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 89794-02-5, its application will become more common.

Some common heterocyclic compound, 89794-02-5, name is 4-Bromo-2-chlorotoluene, molecular formula is C7H6BrCl, 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. Formula: C7H6BrCl

Mg turnings (11.3 g) in a flask with a rubber septum were stirred vigorously under high vacuum for 2-3 h. The flask was filled with N2 and THF (150 mL), then a solution of 4-bromo-2-chloro-toluene (95.7 g, 0.4658 mol) in THF (300 mL) was added starting with 50 mL, then dropwise, while the internal temperature was maintained below 40 0C. The mixture was stirred overnight, then diluted with THF (200 mL) and compoudn T-2 was added slowly. The temperature was maintained under 40 0C using ice and water. Upon completion of addition, stirring was continued at room temperature for 2 h. Then the reaction mixture was poured into NH4Cl (saturated aqueous, 2 L) and adjusted to pH 5 with 2 N HCl (about 300 mL). The organic layer was separated and the aqueous layer was extracted with toluene twice. The combined organic layers were washed with water, then heated at reflux for 4-5 h. Then the mixture volume was reduced to ~50% by atmospheric distillation until the temperature reached 110 0C. The mixture was maintained at reflux for 3 h and stirred at room temperature overnight. Pyridine (35 mL) was added and the mixture was kept at 50 0C for 10 minutes. Crystallization by the addition of heptane afforded compound T-3.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 89794-02-5, its application will become more common.

Reference:
Patent; MERCK & CO., INC.; WO2007/47496; (2007); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics