Analyzing the synthesis route of 3022-15-9

3022-15-9, The synthetic route of 3022-15-9 has been constantly updated, and we look forward to future research findings.

3022-15-9, Piperazine-2-carboxylic acid dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Intermediate 1 Preparation of N,N-Bis-Cbz-2-carboxypiperazine To a mixture of 2-carboxypiperazine dihydrochloride (5.08 g, 25 mmol), 1,3-dioxolane (45 ML), and water (30 ML) at 0 C. was added 50% aqueous sodium hydroxide (NaOH) (6 ML) dropwise.benzyl chloroformate (BzCOCl) (7.8 ML, 55 mmol) then was added to the resulting mixture dropwise in alternating portions with 50% aqueous sodium hydroxide (4 ML) in order to maintain a PH between 8-11.The temperature of the reaction was maintained below 15 C. during a 30-minute addition period.The resulting biphasic mixture was stirred at 0 C. for an additional 30 minutes, after which the reaction was acidified to PH 2 with 2 N hydrochloric acid (HCl), then diluted with ethyl acetate (100 ML).The organic layer was washed with brine (2*10 ML), and the aqueous phase was reextracted with ethyl acetate (20 ML).The combined organic extracts then were dried over sodium sulfate (Na2SO4), filtered, and concentrated under reduced pressure.The residue was purified by flash column chromatography, eluding with methylene chloride/methanol (40:1 to 10:1), to provide the bis-protected piperazine as a white solid (7.0 g, 70%): TLC Rf (10:1 methylene chloride/methanol)=0.55; 1H NMR (300 MHz, DMSO-d6) delta7.40-7.20 (m, 10H), 5.01-5.27 (m, 4H), 4.92-4.60 (m, 2H), 4.20-3.81 (m, 2H), 3.40-2.82 (m, 3H).

3022-15-9, The synthetic route of 3022-15-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Orme, Mark W; Sawyer, Jason Scott; US2003/225093; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics