With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.168646-54-6,5,6-Diamino-1,10-phenanthroline,as a common compound, the synthetic route is as follows.
1) Under a nitrogen atmosphere,4,4′-dimethyldiphenylamine (1.97 g, 10 mmol)CuI (28.5 mg, 0.15 mmol),1,10-phenanthroline (54 mg, 0.3 mmol)Potassium hydroxide (1.12 g, 15 mmol),2-iodo-dithiophene (3.16 g, 12 mmol),Water (7 mL) and xylene (20 mL)The reaction was carried out at 130 ¡ã C for 24 hours,The reaction mixture was poured into methylene chloride (100 mL), washed with water, and the organic phase was collected and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was passed through a silica gel column. The mobile phase was a 1: 3 by volume mixture of dichloromethane and petroleum ether to give intermediate P3;2)The intermediate P3 (3.35 g, 10 mmol) was dissolved in dry dichloromethane (50 mL)Anhydrous aluminum trichloride (1.6 g, 12 mmol) was added portionwise at 0 ¡ã C,After stirring for 20 minutes,A solution of oxalyl chloride (5 mmol) in dichloromethane (10 mL) was slowly added dropwise,Drop finished, rose to room temperature to continue stirring 6 hours, the reaction completed,A 10percent aqueous hydrochloric acid solution (10 mL) was added dropwise to the reaction solution,The organic phases were collected, washed with saturated sodium bicarbonate solution and water, dried over anhydrous sodium sulfate,The solvent was distilled off under reduced pressure,The residue was passed through a silica gel column and the mobile phase was a 1: 1 by volume mixture of dichloromethane and petroleum ether to give intermediate P4;3) 5,6-diamino-1, 10-phenanthroline A (2.10 g, 10 mmol)Intermediate P4 (10 mmol) and glacial acetic acid (40 mL) were refluxed at 120 & lt; 0 & gt; C for 24 hours,Down to room temperature,The solvent was distilled off under reduced pressure,The residue was extracted with chloroform,Washed with 10percent sodium bicarbonate solution and saturated brine, respectively,Dried over anhydrous sodium sulfate.The solvent was distilled off under reduced pressure, the residue was passed through a silica gel column,The mobile phase is a 1: 1 by volume mixture of methylene chloride and ethyl acetate,The organic photosensitive dye D2, the yield of 56percent
168646-54-6, As the paragraph descriping shows that 168646-54-6 is playing an increasingly important role.
Reference£º
Patent; China Academy of Sciences Huaxue Academe; Zhang, Lipeng; Fan, Xinheng; Chen, Qiang; Jiang, Kejian; Yang, Lianming; (14 pag.)CN104672237; (2017); B;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI