548762-66-9, (2S,5R)-tert-Butyl 2,5-dimethylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,548762-66-9
In a round bottom flask, 2-(chloro(4-fluorophenyl)methyl)-3-fluoropyridine (790 mg, 3.30 mmol) was dissolved in acetonitrile (16.5 mL). To this solution, potassium iodide (54.7 mg, 0.330 mmol), triethylamine (0.919 mL, 6.59 mmol) and tert-butyl (2S,5R)-2,5-dimethylpiperazine-1-carboxylate (706 mg, 3.30 mmol) were added sequentially. After heating at 75 C for 5 hours, TLC in 2:3 ethyl acetate/hexanes showed a trace of starting material and two new compounds of lower rf. LSMS was consistent with 2 major products each having the correct MW corresponding to the two separable diastereomers. The crude material was chromatographed on a 24 g silica gel column with 10-50 % ethyl acetate in hexanes to separate two major fractions labeled Isolate-1 and Isolate-02. LCMS showed that each fraction was consistent with a single diastereomer contaminated with a small amount of the other diastereomer. (1453) Intermediate 157: Isolate-1, First eluting fraction. Analytical LCMS conditions: Injection Vol= 1 mL, Start %B 0, Final %B 100, Gradient Time 2 Minutes, Flow Rate 1 mL/min, Wavelength 220 nm, Solvent Pair Acetonitrile/ Water/ TFA, Solvent A 10 % acetonitrile/ 90 % water/ 0.05% TFA, Solvent B 10 Water 90 % acetonitrile/ 0.05% TFA, Column Acquity BEH C1821. X 50 mm 1.7 mm, Oven Temp= 40 C. LCMS results; retention time 1.27 minutes, observed mass 418.5 (MH+). (1454) Intermediate 158: Isolate-2, Second eluting fraction. Analytical LCMS conditions: Injection Vol= 1 mL, Start %B 0, Final %B 100, Gradient Time 2 Minutes, Flow Rate 1 mL/min, Wavelength 220 nm, Solvent Pair acetonitrile/water/TFA, Solvent A 10 % acetonitrile/90 % water/0.05% TFA, Solvent B 10 Water 90 % acetonitrile/0.05% TFA, Column Acquity BEH C1821. X 50 mm 1.7 mm, Oven Temp= 40 C. LCMS results; retention time 1.31 minutes, observed mass 418.1 (MH+).
548762-66-9 (2S,5R)-tert-Butyl 2,5-dimethylpiperazine-1-carboxylate 11745988, apiperazines compound, is more and more widely used in various fields.
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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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