84956-71-8, 2-(tert-Butyl)-4,5-dichloropyridazin-3(2H)-one is a pyridazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,84956-71-8
REFERENCE EXAMPLE 1 Synthesis of 2-tert.-butyl-5-chloro-4-methyl-3(2H)-pyridazinone (starting material) To a solution of 6.0 g (0.25 mol) of magnesium in 50 ml of dry tetrahydrofuran was added dropwise 35.5 g (0.25 mol) of methyl iodide under stream of nitrogen to produce a Grignard reagent. After completion of adding the methyl iodide, 1000 ml of dry toluene was added thereto. The resulting solution was heated to 60 to 70 C. and added dropwise with methyl iodide until the magnesium was completely consumed. The resulting Grignard reagent was cooled to room temperature and was added dropwise over 20 minutes with 22.1 g (0.1 mol) of 2-tert.-butyl-4,5-dichloro-3(2H)-pyridazinone dissolved in 200 ml of dry toluene. After completion of adding, the reaction liquid was subjected to reaction for 1.5 hours at room temperature and then poured into a solution of 100 ml of conc. hydrochloric acid in 900 ml of ice-water to effect extraction. The resulting organic layer was then washed with 500 ml of 10% aqueous solution of sodium hydroxide and then with 500 ml of water, and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to give 17.2 g of a crude product. The crude product was subjected to distillation (boiling point: 60 to 62 C./0.22 mmHg) and then column chromatography (silica gel; hexane_acetone=15:1) for separation and purification to give 4.5 g of 2-tert.-butyl-5-chloro-4-methyl-3(2H)-pyridazinone. ND20 =1.5238. NMR (CDCl3, delta, TMS): 1.63 (9H, s), 2.23 (3H, s), 7.66 (1H, s).
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Reference£º
Patent; Nissan Chemical Industries, Ltd.; US4874861; (1989); A;,
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