With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.84956-71-8,2-(tert-Butyl)-4,5-dichloropyridazin-3(2H)-one,as a common compound, the synthetic route is as follows.
84956-71-8, 2-(t-butyl)-4,5-dichloro-2-hydro-pyridazin-3-one (1.66 g, 7.50 mmol) and (4-(2-methyl-1,3-dioxolan-2-yl)phenyl) methanol (0.971g, 5.00mmol; for example, Takebayashi, S;. Dabral, N;. Miskolzie, M;.. Bergens, S.H.J.Am.Chem.Soc, 2011,133,25, 9666-9669, )solution in dry dimethylformamide (50.0 mL) to a it was treated at ambient temperature at a time by cesium carbonate (3.26g, 10.0mmol). Then, the resulting suspension was immersed in a preheated oil bath , and maintained at 65 C., with vigorous stirring, for 4 hours. After cooling to ambient temperature, the suspension was maintained for a further 12 hours,and then, is transferred to a separation funnel, and ethyl acetate (each 50 ml) and divided into water. Furthermore, these layers are separated, washed with ethyl acetate aqueous layer (2¡Á50mL). A saturated aqueous sodium chloride in combination with ethyl acetate (5¡Á50mL) washing and cleaning, then, dried with magnesium sulfate, filtering, in reduced pressure to concentrate the yellow solid. Subsequently, coarse material, 7:3 hydroxypentanoic/ethyl acetate is purified by using silica chromatography (40¡Á220mm). The main product is recovered at peak 400-700mL eluent, pools, in reduced pressure concd. white solid. Subsequently, the material is purified hot ethyl acetate/aminopentanenitrile by recrystallization from a colorless needle is obtained (1. 33g, 3. 51mmol; 70. 1%).1H NMR : (300MHz, DMSO-d6) delta8. 27 (1H, s), 7. 52-7. 36 (4H, m), 5. 44 (2H, s), 4. 07-3. 93 (2H, m), 3. 76-3. 60 (2H, m), 1. 57 (9H, s), 1. 55 (3H, s).13C NMR : (75MHz, DMSO-d6) delta157. 8,153. 9,143. 6,134. 9,127. 7,126. 2,125. 4,115. 5,107. 9, 71. 2, 65. 4, 64. 1, 27. 5, 27. 2. HRMS C19H2335ClN2O4to calculated value (M+H): 379. 1419 ; measured value: 379. 1416. TLC: Rf0. 39 (silica gel, 7:3 hydroxypentanoic/ethyl acetate, uv).
84956-71-8 2-(tert-Butyl)-4,5-dichloropyridazin-3(2H)-one 2782225, apyridazine compound, is more and more widely used in various fields.
Reference£º
Patent; LANTHEUS MEDICAL IMAGING INCORPORATED; CESATI, RICHARD R; RADEKE, HEIKE S; PANDEY, SURESH K; PUROHIT, AJAY; ROBINSON, SIMON P; (297 pag.)JP2015/531760; (2015); A;,
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