New learning discoveries about 3022-15-9

As the paragraph descriping shows that 3022-15-9 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3022-15-9,Piperazine-2-carboxylic acid dihydrochloride,as a common compound, the synthetic route is as follows.

EXAMPLE-6 2-Cyano-1-(4-isopropyl-2-piperazinyl)-carbonyl Pyrrolidine Trifluoroacetate (Compound No.2). Step-1 To an aqueous (100 ml) sodium hydroxide (4.0 g, 100 mmol) solution of piperazine-2-carboxylic acid dihydrochloride (5 g, 24.63 mmol) is added a solution of di-tert-butyl dicarbonate (11.0 g, 50.45 mmol) in dioxan (50 ml) at 0 C. over a period of half an hour. The reaction mixture is stirred at 0 C. for 1 hr. followed by stirring at room temperature (25 C.) for another 2 hrs. Neutralized (pH 6-7) with aqueous 2N HCl, extracted with ethyl acetate. Organic layer washed with brine solution, dried (Na2SO4) and evaporated in vacuo to yield an oil which solidifies on cooling. (Yield 8.02 g, 98.76%)., 3022-15-9

As the paragraph descriping shows that 3022-15-9 is playing an increasingly important role.

Reference:
Patent; TORRENT PHARMACEUTICALS LTD.; US2004/106802; (2004); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

New learning discoveries about Piperazine-2-carboxylic acid dihydrochloride

3022-15-9, As the paragraph descriping shows that 3022-15-9 is playing an increasingly important role.

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

A solution of di-tert-butyldicarbonate (63 g, 290 mmol) in MeOH (100 mL) was added portionwise to a solution of piperazine-2-carboxyilic acid dihydrochloride (25.0 g, 123 mmol) and triethylamine (48 mL, 340 mmol) in MeOH (150 mL) over 30 minutes. Upon complete addition, the reaction mixture was heated to 50 0C for 2 h. Upon cooling to rt, the reaction mixture was concentrated under reduced pressure. The material was dissolved in water (300 mL) and the solution was brought to pH 2 with 1 M aqueous HCl. This was extracted with EtOAc (4 x 200 mL), and the combined extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure until -100 mL EtOAc remained. The solution was diluted with hexanes (150 mL) and cooled to 0 0C. The resulting solid was collected by filtration, washed with hexanes (2 x) and air- dried. This gave 38.9 g (96%) of the title compound as a white solid. Analytical data: 1H NMR (400 MHz, DMSO-J6) delta 13.02-12.80 (br, IH), 4.50-4.24 (m, 2H)5 3.94-3.72 (br, IH), 3.66 (d, J= 12.8 Hz, IH), 3.22-2.92 (m, 2H), 2.90-2.68 (brs IH), 1.42-1.34, (m, 18H).

3022-15-9, As the paragraph descriping shows that 3022-15-9 is playing an increasingly important role.

Reference£º
Patent; CRITICAL THERAPEUTICS, INC.; WO2007/146066; (2007); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Downstream synthetic route of 3022-15-9

As the paragraph descriping shows that 3022-15-9 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3022-15-9,Piperazine-2-carboxylic acid dihydrochloride,as a common compound, the synthetic route is as follows.,3022-15-9

Piperazine-2-carboxylic acid dihydrochloride (10.0 g, 49.2 mmol) was dissolved in H2O (125 mL) and 1,4-dioxane (200 mL), and the solution was brought to pH 11 with 50% NaOH in H2O. Benzyl chloroformate (14 mL, 98 mmol) was added while maintaining the pH at 11 with 50% NaOH in H2O. After 1 h, an additional portion of benzyl chloroformate (2 mL, 14 mmol) was added. After 30 min, the solution was extracted with Et2O (3 x 100 mL). The aqueous layer was brought to pH 2 with concentrated HCl and extracted with EtOAc (3 x 200 mL). The combined EtOAc extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure to give 18.9 g (96%) of the desired product as a thick oil. The material was used without further purification. LC-MS: RT = 9.250 min; [M+H]+ = 421.1.

As the paragraph descriping shows that 3022-15-9 is playing an increasingly important role.

Reference£º
Patent; CRITICAL THERAPEUTICS, INC.; WO2007/146066; (2007); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of Piperazine-2-carboxylic acid dihydrochloride

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

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3022-15-9,Piperazine-2-carboxylic acid dihydrochloride,as a common compound, the synthetic route is as follows.

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

Downstream synthetic route of 3022-15-9

3022-15-9, As the paragraph descriping shows that 3022-15-9 is playing an increasingly important role.

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

Example 61 (4-Fluoro-phenyl)-f 3- [3- (4-fluoro-phenyl)- [1, 2,4] oxadiazol-5-yl]-4-methyl-piperazin- l-yl}-methanone; 61 (A) Piperazine-1,3-dicarboxylic acid-1-tert-butyl ester To a solution of 2-piperazine-carboxylic acid dihydrochloride (1.0 g, 4.92 mmol) in 20 mL of water/dioxane 1 : 1, NaOH 6N was added to adjust the pH to 11. A solution of BOC-ONS (1.34 g, 5.41 mmol) in dioxane (5 mL) was then added dropwise, while maintaining the pH=l 1 during the addition and the resulting solution was stirred overnight at room temperature. Another 0.134 g of BOC-ONW were added and the reaction mixture was stirred for 2h. The solvent was evaporated under reduced pressure and the residue was diluted with diethyl ether/water (60 mL). The phases were separated and the pH of the aqueous layer was adjusted to 7 by slow addition of HC1 1N. Evaporation of water under reduced pressure afforded the title compound as a white solid which was dried in a vacuum oven at 50C and used without further purification for the next step. LCMS (Tr): 3.3 min (Method B); MS (ES+) gave m/z: 231. 0.

3022-15-9, As the paragraph descriping shows that 3022-15-9 is playing an increasingly important role.

Reference£º
Patent; ADDEX PHARMACEUTICALS SA; WO2005/44797; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics