With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.253-52-1,Phthalazine,as a common compound, the synthetic route is as follows.
To a stirred solution of tert-butyl acetate(2.67 g, 3.08 mL, 23.0 mmol) in dry THF (40 mL) at ?78 ¡ãC was added dropwise n-butyllithium(2.5 M in hexanes, 7.68 mL, 19.2 mmol) over a period of 30 min. The solution was warmed to ?25 ¡ãCand stirred at this temperature for a period of 30 min. To this reaction mixture was added a solution of1 (2.00 g, 15.4 mmol) in dry THF (25 mL), and stirring was continued for an additional 30 min at 0 ¡ãC.The reaction mixture was poured into saturated NH4Cl (100 mL) and extracted with EtOAc (3 ¡Á 50 mL).The organic extracts were washed with saturated NaCl (50 mL), dried (MgSO4) and concentrated toafford 8 as a light brown oil. The crude product 8 was then dissolved in DCM (50 mL), andtriethylamine (1.86 g, 2.56 mL, 18.4 mmol) was added, followed by dropwise addition of acryloylchloride (1.39 g, 1.25 mL, 15.4 mmol) at 0 ¡ãC. The reaction mixture was stirred at 0 ¡ãC for a period of2 h. The reaction was quenched with saturated NaCl (50 mL), and the organic layer was separated. Theaqueous layer was extracted with DCM (2 ¡Á 50 mL) and the combined organic layers were washedwith saturated NaCl (50 mL), dried (MgSO4), filtered, and concentrated to afford the crude product.The crude product was purified on a silica gel column eluted with hexanes?EtOAc (4:1) to afford 9a(4.00 g, 87percent) as a colorless liquid.
The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.
Reference£º
Article; Nammalwar, Baskar; Muddala, N.Prasad; Bourne, Christina R.; Henry, Mary; Bourne, Philip C.; Bunce, Richard A.; Barrow, Esther W.; Berlin, K.Darrell; Barrow, William W.; Molecules; vol. 19; 3; (2014); p. 3231 – 3246;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem