反应详情

To 10 ml of dry N,N-dimethylformamide was added 0.75 g of 55% sodium hydride. The resulting mixture was kept at 0° C. and was added dropwise with a solution of 2.2 g of 2-t-butyl-5-chloro-4-ethyl-3(2H)-pyridazinone dissolved in 15 ml of N,N-dimethylformamide. After ten minutes passed, the resulting mixture was added dropwise with a solution of 1.4 g of p-chlorobenzyl alcohol dissolved in 15 ml of N,N-dimethylformamide. After completion of dropwise addition, the resulting mixture was reacted at 80° C. for one hour. The resulting solution was poured into 50 ml of water and extracted twice with 50 ml of diethyl ether. The resulting organic layer was dried over anhydrous sulfate and freed of solvent by distillation under reduced pressure to give a crude product. The crude product was recrystallized from hexane to obtain 2.4 g of 2-t-butyl-5-(p-chlorobenzyloxy)-4-ethyl-3(2H)-pyridazinone.

1. customwas kept at 0° C.
2. waitAfter ten minutes passed
3. additionAfter completion of dropwise addition
4. customthe resulting mixture was reacted at 80° C. for one hour
5. extractionextracted twice with 50 ml of diethyl ether
6. dry with materialThe resulting organic layer was dried over anhydrous sulfate
7. distillationfreed of solvent by distillation under reduced pressure
8. customto give a crude product
9. customThe crude product was recrystallized from hexane