Synthetic Route of 56961-77-4, These common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, 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.
Intermediate 1:[0114] A well-dried flask was first charged with l-bromo-2,3-dichlorobenzene (4 g, 17.7 mmol) and 1,4-diazepane (2.1 g, 20.9 mmol), which was evacuated and backfilled with N2 through a balloon under gentle warming (40C). Toluene was charged and the mixture was bubbled with N2 for 10 min, then BINAP (318 mg, 0.51 mmol) and Pd2dba3 (156 mg, 0.17 mmol) was added to the mixture, followed by DBU (3.4 mL). The resulting mixture was warmed at 60- 70C while fine powder of tBuONa was added in one portion to start the amination. After the reaction mixture cooled to rt, (Boc)20 (11 g, 51 mmol) solution in DCM was added dropwise to the reaction mixture, then stirred for 3 h at rt. The reaction mixture was diluted with water and extracted with EtOAc. The combined EtOAc layers were washed with brine, dried over anhydrous Na2S04, concentrated in vacuo and purified by flash chromatography on silica gel column (elution with PE/EtOAc = 10:1) to give tert-butyl 4-(2,3-dichlorophenyl)-l,4-diazepane- 1-carboxylate (intermediate 1) (4.1 g, 70%) as a yellow oil.
Statistics shows that 1-Bromo-2,3-dichlorobenzene is playing an increasingly important role. we look forward to future research findings about 56961-77-4.
Reference:
Patent; THE UNIVERSITY OF NORTH CAROLINA AT CHAPEL HILL; JIN, Jian; ROTH, Bryan; FRYE, Stephen; WO2012/3418; (2012); A2;,
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