Reference of 87486-33-7, These common heterocyclic compound, 87486-33-7, name is 3,5-Dichloro-1-methylpyrazin-2(1H)-one, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
General procedure: 6?-Chloro-4?-methyl-4-(2-trifluoromethyl-benzoyl)-3,4,5,6-tetrahydro-2H,4?H-[1,2?]bipyrazinyl-3?-one (1)[0262][0263]Compound 1 is prepared according to synthesis method 1: 1.76 g (5.97 mmoles) of derivative 1 h and 1.13 g (6.31 mmoles) of pyrazinone 4c are placed in 3 ml of butanol-1 in the presence of 4 ml (27.9 mmoles) of NEt3. This mixture is stirred at 120 C. for 24 hours. After concentrating the reaction medium to dryness, the residue obtained is taken up with AcOEt and washed with water and with a saturated NaCl solution. After drying on MgSO4, the organic phase is concentrated to dryness. The residue obtained is purified by silica flash chromatography (CH2Cl2-AcOEt gradient: 100-0 to 90-10). 0.86 g of beige solid is isolated (yield: 36%).[0264]TLC silica gel 60 F 254 Merck, CH2Cl2-MeOH: 95-5, Rf=0.71.[0265]F=162 C.[0266]1H NMR (CDCl3) ppm: 3.28 (t, 2H, J=5.18 Hz), 3.44 (s, 3H), 3.67-3.88 (m, 3H), 3.93-4.09 (m, 3H), 6.73 (s, 1H), 7.35 (d, 1H, J=7.6 Hz), 7.54 (t, 1H, J=7.6 Hz), 7.62 (t, 1H, J=7.6 Hz), 7.73 (d, 1H J=8 Hz).[0267]MS (+ESI) m/z 401 (MH+)
Statistics shows that 3,5-Dichloro-1-methylpyrazin-2(1H)-one is playing an increasingly important role. we look forward to future research findings about 87486-33-7.
Reference:
Patent; PIERRE FABRE MEDICAMENT; Leroy, Isabelle; Dupont-Passelaigue, Elisabeth; Mialhe, Samuel; Junquero, Didier; Valeille, Karine; US2013/40928; (2013); A1;,
Pyrazine – Wikipedia,
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