342405-34-9, The synthetic route of 342405-34-9 has been constantly updated, and we look forward to future research findings.
342405-34-9, 4-(4-Methylpiperazino)benzyl Alcohol is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
To a solution of (4-(4-methylpiperazin-1-yl)phenyl)methanol (103 mg, 0.499 mmol), DIEA (0.131 mL, 0.749 mmol), and DMAP (6.10 mg, 0.050 mmol) in dichloromethane (2.5 mL) at 20 C was added methanesulfonyl chloride (0.058 mL, 0.749 mmol). The reaction mixture was stirred at the same temp while progress was monitored by LCMS. After stirring 24 hours at 20 C, the reaction mixture was concentrated and the resulting material purified by normal phase chromatography (Biotage Isolera, 10 g SNAP ULTRA column, DCM/MeOH) to obtain 123 mg of a brown solid. A portion of this material (27 mg) in N,N- dimethylformamide (0.5 mL) was added to a suspension of 4-ethyl-2-mercapto-6-(4-methyl- 1,4-diazepan-1-yl)pyridine-3,5-dicarbonitrile (synthesis described in Example 69, step 1, 46 mg, 0.122 mmol) and Et3N (0.017 mL, 0.122 mmol) in N,N-dimethylformamide (0.5 mL) at 0 C The reaction mixture was then stirred at 0 C overnight. After stirring overnight at 0 C, the reaction mixture was warmed to room temperature. The reaction mixture was filtered. The filtrate was purified by reverse phase HPLC (Gilson, 30 mm x 50 mm Gemini Column, NH4OH modifier) then re-purified by reverse phase HPLC (Gilson, 30 mm x 50 mm Gemini Column, NH4OH modifier) to obtain 4-ethyl-2-(4-methyl-1,4-diazepan-1-yl)-6- ((4-(4-methylpiperazin-1-yl)benzyl)thio)pyridine-3,5-dicarbonitrile (6 mg) as a yellow oil LCMS m/z = 490.4 [M+H]+.1H NMR (400 MHz, METHANOL-d4) delta ppm 7.26-7.30 (m, J=8.62 Hz, 2H), 6.92-6.97 (m, 2H), 4.44 (s, 2H), 3.95-4.03 (m, 4H), 3.18-3.24 (m, 4H), 2.91 (q, J=7.60 Hz, 2H), 2.76-2.80 (m, 2H), 2.62-2.67 (m, 6H), 2.38 (s, 3H), 2.37 (s, 3H), 2.04-2.11 (m, 2H), 1.31 (t, J=7.60 Hz, 3H).
342405-34-9, The synthetic route of 342405-34-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; ADAMS, Nicholas David; BENOWITZ, Andrew B.; RUEDA BENEDE, Maria Lourdes; EVANS, Karen Anderson; FOSBENNER, David T.; KING, Bryan Wayne; LI, Mei; MILLER, William Henry; REIF, Alexander Joseph; ROMERIL, Stuart Paul; SCHMIDT, Stanley J.; WIGGALL, Kenneth; (1283 pag.)WO2017/216726; (2017); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics