With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.129799-08-2,1-tert-Butyl 3-methyl piperazine-1,3-dicarboxylate,as a common compound, the synthetic route is as follows.
To a stirred solution of 1-(tert-butyl) 3-methyl piperazine-1,3-dicarboxylate (250 mg, 1.023 mmol) in acetonitrile (8 mL) were added DIPEA (0.536 mL, 3.07 mmol) and 4,4′-(bromomethylene)bis(chlorobenzene) (485 mg, 1.535 mmol). The reaction mixture was heated up to 85 C over 10 min and was stirred for 16 h. The reaction mixture was concentrated under high vacuum to yield a brown gum. The crude compound was purified by ISCO (using 24 g silica gel column; using 8 % -12 % ethyl acetate/ petroleum ether) to yield 1-(tert-butyl) 3-methyl 4-(bis(4-chlorophenyl)methyl) piperazine-1,3-dicarboxylate (280 mg, 57.1 % yield) as a brown gum. LCMS: m/z = 481.2 (M+2H); rt 1.803 min; LC-MS Method: Column-KINETEX-XB-C18 (75 x 3 mm- 2.6 ^m); Mobile phase A: 10 mM ammonium formate in water: acetonitrile (98:2); Mobile phase B: 10 mM ammonium formate in water: acetonitrile (2:98); Gradient: 80 % B over 0.5 minute, 80-98% B over 2.5 minutes, flow rate 1.0 mL/min, then a 1 minute hold at 98% B flow rate 1.0 mL/min, 129799-08-2
As the paragraph descriping shows that 129799-08-2 is playing an increasingly important role.
Reference£º
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;,
Piperazine – Wikipedia
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