Sep 2021 News Some tips on 1-Ethylpiperazine-2,3-dione

The synthetic route of 59702-31-7 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.59702-31-7,1-Ethylpiperazine-2,3-dione,as a common compound, the synthetic route is as follows.,59702-31-7

1- (4-bromobutyl) -5-benzyloxy-2- (4-benzyloxy-phenyl) -3-methyl -1H- indole (1.0g, 1.8mmol), 1- ethyl piperazine-2,3-dione (0.5g, 3.6mmol), triethylamine (0.4g, 3.6mmol) placed in 100mL eggplant flask, n-butanol as solvent, the reaction was refluxed for 4h. Rotary evaporation. The residue was mixed with ethyl acetate and dissolved in ethanol, was added 10% Pd / C (0.2g, 0.4mmol), 45 reaction 24h. Filtered off Pd / C, the filtrate by rotary evaporation, column chromatography, as a white oil 0.22g, yield 49.1%

The synthetic route of 59702-31-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shenyang Pharmaceutical University; Hu, Chun; Liu, Xiaoping; Zuo, Li; Huang, Erfang; Zhang, Lan; Jin, Zhe; (11 pag.)CN105801564; (2016); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Downstream synthetic route of 59702-31-7

59702-31-7 1-Ethylpiperazine-2,3-dione 108812, apiperazines compound, is more and more widely used in various fields.

59702-31-7, 1-Ethylpiperazine-2,3-dione is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

500 ml of ethylene glycol dimethyl ether and 28.4 g of 4-ethyl-2,3-bisperoxazine were sequentially added to a 1 L three-necked flask, and the mixture was evenly stirred. 4.6 g of sodium metal was added and the mixture was heated to reflux for 10 hours.Cooled to 5 C,Stirring in batches by adding a good configuration of the triphosgene solution,The reaction temperature was controlled not to exceed 10 C,Adding filtrate to remove the activated carbon, filter to remove activated carbon, the filtrate vacuum drying, drying, in a white solid, that is, N, N, N-dimethylformamide, N, N-dimethylformamide, Carbonyl-bis- (4-ethyl-2,3-bisperoxypyrazine) was obtained The preparation method was the same as that of Example 1 except that the reaction temperature of sodium bisoxypiperazine and triphosgene was -15 C, and the obtained N, N’-carbonyl-bis- (4-ethyl- Piperazine)The yield of 4-ethyl-2,3-bisperoxypiperazine was 95%. The purity was 98.5% by HPLC., 59702-31-7

59702-31-7 1-Ethylpiperazine-2,3-dione 108812, apiperazines compound, is more and more widely used in various fields.

Reference:
Patent; Shandong Ai Fu Special Technology Co., Ltd.; Gao, Aihong; Feng, Weichun; Zhang, Jianwen; Ji, Xiaohong; Liu, Lixiu; Liu, Maoling; Wang, Liqin; (6 pag.)CN105524001; (2016); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Downstream synthetic route of 59702-31-7

59702-31-7 1-Ethylpiperazine-2,3-dione 108812, apiperazines compound, is more and more widely used in various fields.

59702-31-7, 1-Ethylpiperazine-2,3-dione is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

500 ml of ethylene glycol dimethyl ether and 28.4 g of 4-ethyl-2,3-bisperoxazine were sequentially added to a 1 L three-necked flask, and the mixture was evenly stirred. 4.6 g of sodium metal was added and the mixture was heated to reflux for 10 hours.Cooled to 5 C,Stirring in batches by adding a good configuration of the triphosgene solution,The reaction temperature was controlled not to exceed 10 C,Adding filtrate to remove the activated carbon, filter to remove activated carbon, the filtrate vacuum drying, drying, in a white solid, that is, N, N, N-dimethylformamide, N, N-dimethylformamide, Carbonyl-bis- (4-ethyl-2,3-bisperoxypyrazine) was obtained The preparation method was the same as that of Example 1 except that the reaction temperature of sodium bisoxypiperazine and triphosgene was -15 C, and the obtained N, N’-carbonyl-bis- (4-ethyl- Piperazine)The yield of 4-ethyl-2,3-bisperoxypiperazine was 95%. The purity was 98.5% by HPLC., 59702-31-7

59702-31-7 1-Ethylpiperazine-2,3-dione 108812, apiperazines compound, is more and more widely used in various fields.

Reference:
Patent; Shandong Ai Fu Special Technology Co., Ltd.; Gao, Aihong; Feng, Weichun; Zhang, Jianwen; Ji, Xiaohong; Liu, Lixiu; Liu, Maoling; Wang, Liqin; (6 pag.)CN105524001; (2016); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

New learning discoveries about 1-Ethylpiperazine-2,3-dione

59702-31-7 1-Ethylpiperazine-2,3-dione 108812, 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.59702-31-7,1-Ethylpiperazine-2,3-dione,as a common compound, the synthetic route is as follows.,59702-31-7

(2)–To a suspension of 0.71 g of the abovementioned 1-ethyl-2,3-dioxo-piperazine in 15 ml of anhydrous dioxane were added with stirring 0.70 g of trimethylsilyl chloride and 0.83 ml of triethylamine. The resulting mixture was stirred at room temperature for 20 hours to deposit triethylamine hydrochloride. This hydrochloride was separated by filtration, and the filtrate was dropped at 5 to 10 C. into a solution of 0.70 g of phosgene in 10 ml of anhydrous tetrahydrofuran. Subsequently, the resulting mixture was reacted at 5 to 10 C. for 30 minutes and at room temperature for 2 hours, and then the solvent was removed by distillation under reduced pressure to obtain 1.0 g of pale yellow crystals of 4-ethyl-2,3-dioxo-1-piperazinocarbonyl chloride. IR (KBr) cm-1: — nuC=O 1780, 1660

59702-31-7 1-Ethylpiperazine-2,3-dione 108812, apiperazines compound, is more and more widely used in various fields.

Reference:
Patent; Toyama Chemical Co., Ltd.; US4112090; (1978); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of 59702-31-7

The synthetic route of 59702-31-7 has been constantly updated, and we look forward to future research findings.

59702-31-7, 1-Ethylpiperazine-2,3-dione is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

59702-31-7, 650 L of dichloromethane was pumped into a 1000 L No. 2 dissolution tank, and 89 kg of ethyl-dioxypiperazine was added to the feed port under vacuum to cool to 5 C. 91 kg of trimethylchlorosilane was vacuumed in, stirred for 30 min, and the temperature was further lowered to 0 C to obtain a first intermediate.

The synthetic route of 59702-31-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Changzhou Hong Sun Pharmaceutical Co., Ltd.; Chen Jianlin; Zhang Xuejiao; (17 pag.)CN109438476; (2019); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 1-Ethylpiperazine-2,3-dione

As the paragraph descriping shows that 59702-31-7 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.59702-31-7,1-Ethylpiperazine-2,3-dione,as a common compound, the synthetic route is as follows.,59702-31-7

Step A (4-Ethyl-2,3-dioxo-piperazin-1-yl) -acetic Acid To a solution of N-ethylpiperazin-2,3-dione (1.0 g, 7.0 mmol) in 10 mL of t-butanol over ice is added solid K2CO3 (1.1 g, 8.0 mmol). After stirring a few minutes t-butylbromoacetate (1.2 mL, 8.1 mmol) is introduced dropwise. The resultant mixture is stirred overnight at ambient temperature. The t-butanol is then azeotroped off with cyclohexane and the residue is partitioned between EtOAc and brine. The phases are separated and the organic phase is extracted 2*1M HCl, 2*saturated NaHCO3, and 2*brine; dried over Na2SO4; and concentrated to give the ester as a white solid (0.35 g, 1.4 mmol, 19%).

As the paragraph descriping shows that 59702-31-7 is playing an increasingly important role.

Reference£º
Patent; Gailunas, Andrea; Tucker, John A.; TenBrink, Ruth; Mickelson, John; US2003/109559; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of 59702-31-7

The synthetic route of 59702-31-7 has been constantly updated, and we look forward to future research findings.

59702-31-7, 1-Ethylpiperazine-2,3-dione is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

59702-31-7, EXAMPLE 6 1-Ethyl-4-(mercaptomethyl)-Piperazine-2,3-dione To a solution of 1-ethylpiperazine-2,3-dione (2.13 g, 15 mmol) in 30% aqueous (methanol free) formaldehyde (15 mmol) potassium hydroxide (150 mg, 2.7 mmol) was added and the mixture stirred at 50 C. for 7 days. It was neutralized with 5 N aqueous hydrochloric acid (50 mul) to pH=7. The mixture was evaporated at 15 mm and then dried in high vacuo (0.0013 mbar) (0.001 mm) to give 1-ethyl-4-(hydroxymethyl)-piperazine-2,3-dione as a colourless solid (100%). NMR-spectrum in CDCl3: 1.15 (broad signal, 1H), 1.15 (t, 3H, J=7 Hz), 3.47 (q, 2H, J=7 Hz), 3.54 (m, 2H), 3.68 (m, 2H), 4.88 (s, 2H) ppm.

The synthetic route of 59702-31-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Pfaendler, Hans Rudolf; US2001/31749; (2001); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 59702-31-7

As the paragraph descriping shows that 59702-31-7 is playing an increasingly important role.

59702-31-7, 1-Ethylpiperazine-2,3-dione is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a four-necked flask was added 4-ethyl-2,3-dioxopiperazine (14.2 g, 0.1 mol)Dichloromethane (60 ml) and trimethylchlorosilane (13.0 g, 0.12 mol) were added. The temperature was controlled to -10 to -20 C. and triethylamine (25.5 g, 0.25 mol) was added dropwise to -5 to 0, Stirring for 12min;Ethyl-2,3-dioxopiperazine chloride (22.4 g, 0.11 mol) was dissolved in 20 ml of methylene chloride,The temperature was controlled at 0 C ~ -5 C for 40min, warmed to 25 C and incubated for 8h. After the reaction was completed, the temperature was lowered to -15 C, filtered and the filter cake was rinsed with precooled dichloromethane (8ml). The mother liquor was combined and concentrated (30 ~ 40 , the degree of vacuum is <0.1MPa) to obtain crude product 0.4g (yield 98.6%, purity 95%)., 59702-31-7

As the paragraph descriping shows that 59702-31-7 is playing an increasingly important role.

Reference£º
Patent; Jiangxi Fuxiang Pharmaceutical Co., Ltd.; Zheng Yuyi; Wu Xiaofeng; Zhou Zhongbo; Xie Yongju; Wang Dongdong; (8 pag.)CN104529914; (2017); B;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 59702-31-7

As the paragraph descriping shows that 59702-31-7 is playing an increasingly important role.

59702-31-7, 1-Ethylpiperazine-2,3-dione is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

59702-31-7, 100 mg (0.32 mmol) of 5,5′-diallyl-3- (chloromethyl)-[1,1′-biphenyl] -2,2′-diol (Intermediate 4),54mg (0.38mmol) of N-ethyl-2,3-diketopiperazine,140.44mg (0.43mmol) of cesium carbonate, a catalytic amount of potassium iodide was added to a 10ml round bottom flask, acetonitrile was added to dissolve, heated to 80 C, and reacted overnight. After the reaction was completed, the reaction solution was cooled to room temperature, and then poured into water. Extracted with ethyl acetate, washed with saturated brine, dried over anhydrous sodium sulfate, spin-dried, and passed through a column (dichloromethane-methanol = 20/1) to obtain 42 mg of a yellow powdery solid with a yield of 31.1%.

As the paragraph descriping shows that 59702-31-7 is playing an increasingly important role.

Reference£º
Patent; Sichuan University; Chen Lijuan; Wei Yuquan; Ye Haoyu; (42 pag.)CN110343033; (2019); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Downstream synthetic route of 59702-31-7

59702-31-7 1-Ethylpiperazine-2,3-dione 108812, apiperazines compound, is more and more widely used in various fields.

59702-31-7, 1-Ethylpiperazine-2,3-dione is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,59702-31-7

Example 48 5-chloro-N-((1-(4-(4-ethyl-2,3-dioxopiperazin-1-yl)phenyl)-1H-imidazol-4-yl)methyl)thiophene-2-carboxamide (60) A mixture of 5-chloro-N-((1-(4-iodophenyl)-1H-imidazol-4-yl)methyl)thiophene-2-carboxamide 1-6 (70 mg, 0.16 mmol), N-ethylpiperazine-2,3-dione (45 mg, 0.32 mmol), N,N’-dimethylethylenediamine (0.020 mL, 0.19 mmol) and K2CO3 (65 mg, 0.47 mmol) in DMSO (1 mL) and dioxane (1 mL) was degassed with Ar before being charged with CuI (20 mg, 0.10 mmol). The mixture in a sealed tube was heated at 110 C. overnight. The mixture was then purified by HPLC to give the titled compound (10 mg). MS 458.1 and 460.1(M+H, Cl pattern).

59702-31-7 1-Ethylpiperazine-2,3-dione 108812, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; Millennium Pharmaceuticals, Inc.; US2007/259924; (2007); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics