129799-08-2, 1-tert-Butyl 3-methyl piperazine-1,3-dicarboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
To a solution of 4,4′-(chloromethylene)bis(fluorobenzene) (1.5 g, 6.29 mmol) in acetonitrile (15 mL) was added 1-(tert-butyl) 3-methyl piperazine-1,3-dicarboxylate (1.842 g, 7.54 mmol), followed by DIPEA (3.29 mL, 18.86 mmol). The reaction mixture was stirred at 85 C overnight. The reaction mixture was concentrated under reduced pressure to remove the volatiles and the residue was dissolved in ethyl acetate (150 mL) and washed with water. The aqueous layer was back-extracted with ethyl acetate (100 mL x 2). The combined organic layer was washed with brine, dried over Na2SO4, filtered and the filtrate was concentrated under reduced pressure to give the crude product. The crude residue was purified via silica gel chromatography on ISCO (5-10 % (0493) EtOAc/petroleum ether; 40 g column) to afford the 1-(tert-butyl) 3-methyl 4-(bis(4- fluorophenyl)methyl)piperazine-1,3-dicarboxylate (2.15 g, 4.82 mmol, 77 % yield). (0494) LCMS: m/z = 447.4 (M+H); rt 2.16 min. (LCMS Method: Column: Waters Acquity UPLC BEH C18 (2.1 x 50 mm) 1.7 mm, Mobile phase A: 10 mM ammonium (0495) acetate:acetonitrile (95:5); Mobile phase B: 10 mM ammonium acetate:acetonitrile (5:95), Gradient = 20-90 % B over 1.1 minute, then a 0.6 minute hold at 90 % B; Temperature: 50 C; Flow rate: 0.7 mL/min; Detection: UV at 220 nm)., 129799-08-2
129799-08-2 1-tert-Butyl 3-methyl piperazine-1,3-dicarboxylate 2756819, apiperazines compound, is more and more widely used in various fields.
Reference：
Patent; BRISTOL-MYERS SQUIBB COMPANY; VELAPARTHI, Upender; CHUPAK, Louis S.; DARNE, Chetan Padmakar; DING, Min; GENTLES, Robert G.; HUANG, Yazhong; KAMBLE, Manjunatha Narayana Rao; MARTIN, Scott W.; MANNOORI, Raju; MCDONALD, Ivar M.; OLSON, Richard E.; RAHAMAN, Hasibur; JALAGAM, Prasada Rao; ROY, Saumya; TONUKUNURU, Gopikishan; VELAIAH, Sivasudar; WARRIER, Jayakumar Sankara; ZHENG, Xiaofan; TOKARSKI, John S.; DASGUPTA, Bireshwar; REDDY, Kotha Rathnakar; RAJA, Thiruvenkadam; (0 pag.)WO2020/6018; (2020); A1;,
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