3,3'-(5-bromo-1,3-phenylene)dipyridine synthesis
- Product Name:3,3'-(5-bromo-1,3-phenylene)dipyridine
- CAS Number:1030380-36-9
- Molecular formula:C16H11BrN2
- Molecular Weight:311.18
Yield:1030380-36-9 85.4%
Reaction Conditions:
with tetrakis(triphenylphosphine) palladium(0);potassium carbonate in tetrahydrofuran at 80; for 15 h;Inert atmosphere;
Steps:
1.1
(1) in 250mL three-necked flask,Purged with nitrogen,0.04mol raw material 1,3,5-tribromobenzene,100 ml of THF,0.1 mol 3-pyridine boronic acid,0.0008 mol tetrakis (triphenylphosphine) palladium,Stirring,Then 0.12 mol of K2CO3 aqueous solution (2M) was added,Heated to 80 ° C,The reaction was refluxed for 15 hours,Sample board, the reaction was complete.The mixture was naturally cooled and extracted with 200 ml of dichloromethane. The layers were separated and the extract was dried over anhydrous sodium sulfate and filtered. The filtrate was rotary evaporated and purified over a silica gel column to give Intermediate C1 with an HPLC purity of 99.7% and a yield of 85.4%.
References:
CN106946853,2017,A Location in patent:Paragraph 0054; 0055; 0056
