3,3',4,5-TETRACHLOROBIPHENYL synthesis
- Product Name:3,3',4,5-TETRACHLOROBIPHENYL
- CAS Number:70362-49-1
- Molecular formula:C12H6Cl4
- Molecular Weight:291.99
Yield:-
Reaction Conditions:
with tetrakis(triphenylphosphine) palladium(0);sodium carbonate in water;toluene at 80;Inert atmosphere;Suzuki Coupling;
Steps:
General Procedure for Preparation of PCBs
General procedure: Phenylboronic acid (1 mmol,1 equiv), halogenated benzene (1 mmol, 1 equiv), Pd (PPh3)4 (23.1 mg, 0.02 mmol, 0.02 equiv), 1.6 ml of 2 M sodium carbonate and 3 ml of toluene were added to an oven-dried flask under a nitrogen atmosphere. The reaction mixture was stirred under 80 oC in oil bath for 22 h under a nitrogen atmosphere. When the reaction was complete and cooled to room temperature, the reaction mixture was washed with ethyl acetate (10 mL) and water (10 mL) three times. Then the organic layer was dried over MgSO4 filtered and concentrated in vacuo. The crude product was purified by column chromatography (petroleum ether 60-90 oC) on silica gel to afford pure PCBs.
References:
Xiang, Zhihao;Huang, Shiqing;Zhao, Liang-Liang;Zhang, Zengyu;Chen, Ke;Cao, Wanqiang;Zheng, Keyu;Yan, Xiaoyu [Tetrahedron Letters,2022,vol. 110,art. no. 154200] Location in patent:supporting information