Category: 3022-15-9

Some tips on 3022-15-9

3022-15-9 Piperazine-2-carboxylic acid dihydrochloride 2723757, apiperazines compound, is more and more widely used in various fields.

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

Method-B [0556] Alternatively the above prolinamide derivative can be prepared by the following method. [0557] DIEA (1.35 g, 10.46 mmol), HOBT (1.40 g, 10.37 mmol) sequentially added to piperazine acid (3.30 g, 10 mmol) and L-prolinamide (1.14 g, 10 mmol) in DCM (40 ml) at 0 C. A solution of DCC (2.40 g, 11.65 mmol) in DCM (30 ml) is added slowly at 0 C. over a period of 1 hr. Stirred another 1 hr. at 0 C. and then at 25 C. for 14 hrs. Filtered, DCM distilled off, diluted with ethyl acetate, washed sequentially with saturated aqueous solution of NaHCO3 and brine. Organic layer dried (Na2SO4), evaporated in vacuo purified by column chromatography (ethyl acetate). (Yield 2.6 g, 61.03%).

3022-15-9 Piperazine-2-carboxylic acid dihydrochloride 2723757, apiperazines compound, is more and more widely used in various fields.

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

Simple exploration of 3022-15-9

3022-15-9, 3022-15-9 Piperazine-2-carboxylic acid dihydrochloride 2723757, apiperazines compound, is more and more widely used in various fields.

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, 3022-15-9 Piperazine-2-carboxylic acid dihydrochloride 2723757, apiperazines compound, is more and more widely used in various fields.

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

Brief introduction of 3022-15-9

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.

Piperazine-2-carboxyilc acid dihydrochloride (15.0 g, 73.9 mmol) was dissolved in H2O (240 mL) and 1,4-dioxane (360 mL), and the solution was brought to pH 10 with 6 N NaOH in H2O. Di-tert-butyldicarbonate (28.3 g, 162 mmol) was added while maintaining the pH at 10 with 6 N NaOH in H2O. After 2 h, the reaction mixture was extracted with Et2O (3 x 200 mL). The aqueous layer was brought to pH 3 with 6 N HCl and was extracted with EtOAc (4 x 300 mL). The combined EtOAc extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure to give 14.45 g (59%) of the desired product as an off- white solid. The material was used without further purification. LC-MS: RT = 8.16 min; [M+Na]+ = 353.1.

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

Brief introduction of 3022-15-9

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.

Step A. To a solution of piperazine-2-carboxylic acid dihydrochloride (10 g, 49 mmol) in 40 ml water was added an aqueous solution of sodium hydroxide (39 ml, 2.5 N). A solution of copper (II) sulfate (6.5 g, 26 mmol) in 80 ml water was added, and the deep blue solution was cooled to 5 C. Sodium bicarbonate (5 g, 59 mmol) was added in one portion, followed by the dropwise addition of benzylchloroformate (7.7 ml, 54 mmol) in 40 ml dioxane over 10 minutes. Sodium bicarbonate was added as needed to maintain a basic solution. The reaction was allowed to warm to rt and was stirred for 16 h. The precipitate was filtered and dried to afford 4-carbobenzyloxypiperazine-2-carboxylic acid, copper chelate residue used directly in the next step.

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

Reference£º
Patent; Robichaud, Albert; Mitchell, Ian S.; Lee, Taekyu; Chen, Wenting; US2002/177596; (2002); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 3022-15-9

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.

CuCO3.Cu(OH)2.H2O (15.8 g) was added to the H2O (275 mL) solution of piperazine-2-carboxylic acid, dihydrochloride (22.3 g), then the mixture was refluxed and stirred for 10 min. The insoluble material was filtered off and was washed with hot H2O (165 mL). The filtrate was cooled to room temperature, and NaHCO3 (9.2 g) and 1,4-dioxane (220 mL) was added to the dark blue solution. The mixture was cooled to 0 C. and NaHCO3 (18.5 g) and 50% solution of 4-nitrobenzyl chloroformate in 1,4-dioxane (61.7 g) was added to the mixture for 0.5 h. After stirring for additional 1.5 h at 0 C., the precipitate was filtered and washed with cold H2O (140 mL), EtOH (100 mL), acetone (200 mL) and Et2O (100 mL), then it was allowed to dry under reduced pressure to obtain the pale blue crystals. The crystals were added to the 1 mol/L HCl (330 mL) solution of EDTA.2Na (20.5 g) for 30 min, and stirred for 2 h at room temperature. The suspension was filtered and the filtered material was diluted with EtOH-H2O (7:3, 550 mL) and refluxed for 10 min. The reaction mixture was filtered to obtain the colorless crystals. The recrystallization from the filtrate was carried out 3 times to obtain additional crystals. The combined crystals were dried under reduced pressure to obtain the titled compound (26.25 g, 77%) as colorless crystals. 1H NMR (D2O) delta 2.54-2.61 (m, 1H), 2.89 (dt, 2H, J=12.7, 3.4 Hz), 2.97 (br, 1H), 3.13 (br, 1H), 3.62-4.04 (m, 2H), 5.16 (s, 2H), 7.49 (d, 2H, J=8.6 Hz), 8.14 (d, 2H, J=8.6 Hz).

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

Reference£º
Patent; Wyeth; US2006/276445; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics