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.
crude oil thus obtained in dry dimethylformamide (5.00 mL) then 2-(t-butyl)-4,5-dichloro-2-hydropyridazin-3-one (0.166 g, 0.750 mmol) and cesium carbonate (0.326,1.00mmol ) it was treated at ambient temperature, each one time. Then, the resulting suspension was immersed in an oil bath , with vigorous stirring, and maintained for 21 hours at 65 C.After cooling to ambient temperature, a funnel suspension is separated and transferred to the water and ethyl acetate (each 20 ml) divided into, a separating layer. Next, the washing and drying (2¡Á20mL) ethyl acetate, ethyl acetate aqueous layer in combination with magnesium sulfate, filtration, the amber color of the concentrated oil under reduced pressure. Subsequently, coarse material, 7:3 hydroxypentanoic/ethyl acetate is used, is purified by using silica chromatography (30¡Á180mm). 200-350mL peak elution of the collecting main product, pools, in reduced pressure to concentrate the white solid (0. 191g, 0. 400mmol; 79. 9%).1H NMR : (300MHz, CDCl3) delta7. 71 (1H, s), 7. 15 (1H, d, J = 1. 9Hz), 6. 92 (1H, d, J = 2. 0Hz), 5. 21 (2H, s), 4. 74 (2H, dt, J = 47. 1, 5. 9Hz), 4. 13 (2H, t, J = 6. 0Hz), 3. 86 (3H, s), 2. 17 (2H, dtt, J = 25. 5, 6. 0, 6. 0Hz), 1. 64 (9H, s).13C NMR : (75MHz, CDCl3) delta158. 9,154. 1,153. 4,145. 8,131. 9,125. 0,123. 2,118. 6,118. 0,110. 2, 81. 0 (d, JCF= 164Hz), 71. 0, 68. 9 (d, JCF= 5. 5Hz), 66. 5, 56. 1, 31. 3 (d, JCF= 20. 2Hz), 27. 8. HRMS C19H2379Br35ClN2O4to calculated value (M+H): 477. 0587 ; measured value: 477. 0589. TLC: Rf0. 15 (silica gel, 4:1 hydroxypentanoic/ethyl acetate, CAM).
84956-71-8 2-(tert-Butyl)-4,5-dichloropyridazin-3(2H)-one 2782225, apyridazine compound, is more and more widely used in various.
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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