Category: 496-46-8

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 496-46-8 as follows. Recommanded Product: 496-46-8

Preparation tetranitro glycoluril: equipped with a reflux condenser, a thermometer, a stirrer, pressure-equalizing dropping funnel, the reaction 3000ml four-necked round flask, 500ml of fuming nitric acid.When the temperature to about 10 , 20g glycoluril added rapidly, stirred to dissolution, to give glycoluril – fuming nitric acid solution; the glycoluril – nitric acid solution is sent down to the temperature of the smoke 0 ~ 5 , 250ml of acetic anhydride was added dropwise, drops added maintaining the temperature at 0 ~ 5 ; acetic anhydride addition was completed, the nitration temperature is maintained at 0 ~ 5 , nitration reaction after 4h, the temperature raised to nitration 5 ~ 10 , 3H continued nitration; nitrated using a temperature gradient to gradually warm ,, 5 gradient for 2 hours and then raised 5 , nitration began maintaining the temperature at 0 deg.] C, nitration reaction 2h, 5 increased, i.e., the temperature was raised 5 nitration, nitration continued 2h, then increased 5 , i.e. nitration temperature was raised to 10 , maintained for 3 hours.10min nitration reaction bottle with a precipitate beginning, gradually warming nitration temperature gradient, the amount of precipitation as the reaction temperature, the reaction time increased, the precipitation was complete, the reaction mixture was lowered vial -10 ~ 0 , the reaction was stopped, the bottle within fritted funnel mixture was filtered, the white solid was washed with tetranitromethane glycoluril dichloromethane to large neutral stand soaked in dichloromethane

According to the analysis of related databases, 496-46-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hubei Aerospace Institute of Chemical Technology, CASC; Ha, HengXin; (8 pag.)CN105777575; (2016); A;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Reference of 496-46-8, These common heterocyclic compound, 496-46-8, name is Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A mixture of glycoluril (500 g, 3.51 mol) and paraformaldehyde (105 g, 3.51 mol) in HCl (8 M, 70 mL) was heated at 50 C for 48 h. The reaction mixture was cooled and filtered. The solid was washed with water (500 mL) and then recrystallized with TFA (1.5 L) to yield Glycoluril Dimer as a white solid (334 g, 62 %).

Statistics shows that Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione is playing an increasingly important role. we look forward to future research findings about 496-46-8.

Reference:
Patent; UNIVERSITY OF MARYLAND, COLLEGE PARK; THE GENERAL HOSPITAL CORPORATION; ISAACS, Lyle, David; EIKERMANN, Matthias; CUSIN, Cristina; COTTEN, Joseph; (128 pag.)WO2016/61571; (2016); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Synthetic Route of 496-46-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 496-46-8, name is Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

tetraallylglycoluril A three-neck 100 ml flask was flushed with argon. Anhydrous DMSO (40 ml) was added and glycoluril (1.42 g, 10 mmol) was dissolved. Then potassium tert-butoxide (5.62 g, 50 mmol) was gradually added and the mixture was further stirred for 1.0 h. Allyl bromide (7.0 ml, 80 mmol) was injected into the reaction mixture and the reaction was performed at 25C for 20 h. 500 ml aqueous solution of HCl (0.1 M) was added into the reaction mixture. 100 ml ethyl acetate was used to extract the mixture andthe organic phase was washed by saturated NaCl aqueous solution(100 ml) for three times. After being dried by MgSO4, the solventwas removed. 1.53 g target product was obtained after purifica-tion over silica column with the eluent of ethyl acetate/petroleumether (60-90C) (v/v, 3:2). All procedures were performed in argonatmosphere.

The synthetic route of Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chen, Bingfeng; Li, Fengbo; Huang, Zhijun; Lu, Tao; Yuan, Guoqing; Applied Catalysis A: General; vol. 481; (2014); p. 54 – 63;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Reference of 496-46-8, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 496-46-8 as follows.

Synthesis of cucurbit[n]urils in methanesulphonic acid using Diethoxymethane(Ethylal)Unsubstituted glycoluril (19.94 g) and methane sulphonic acid (neat, 82 mL) were placed in a reaction flask and heated to 80 C. Ethylal (35.21 mL) was added in drop-wise and the reaction mixture was then heated to 100 C (internal temp) for 18 hours. The reaction mixture was cooled and added to acetone (410 ml) to produce a brown powder which was analysed by1H NMR.Approximate Yields b1H NMR (% of recovered product) cucurbii[5]urii 8%, cucurbit[6]uri 42%, cucurbit[7]uril 43%, cucurbit[8]uril 7%, cucurbit[9]uril 0%, cucurbit[10]uril 0%, cucurbit[ 13uril 0%.Residual formaldehyde by HPLC method was 34 ppm.

According to the analysis of related databases, 496-46-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AQDOT LIMITED; COULSTON, Roger; DIEC, David; NOGUEIRA, Guilherme; GERARDUS DE ROOIJ, Johannes; (23 pag.)WO2018/115822; (2018); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 496-46-8 as follows. name: Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione

A suspension of 28.4 g (0.2 mol) of glycoluril 1 and 80 g of 40% formaldehyde solution was alkalized with a 20% NaOH solution to 9-10, after which the mixture was stirred at 50 C for 2 h. 70% of water was distilled off, and tetra-N-hydroxymethyl glycoluril was separated and washed with acetone. Yield of 2 26.2 g (50%), mp 136.5 C. IR spectrum(KBr), nu, cm-1: 1718.31 (=), 3337.39 (). 1H NMR spectrum (400 MHz, DMSO), delta, ppm: 5.47 s(2H, CH), 4.62-4.79 m (8H, CH2).

According to the analysis of related databases, 496-46-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Sal?keeva; Bakibaev; Khasenova; Taishibekova, Ye. K.; Sugralina; Minaeva, Ye. V.; Sal?keeva; Russian Journal of Applied Chemistry; vol. 89; 1; (2016); p. 132 – 139; Zh. Prikl. Khim. (S.-Peterburg, Russ. Fed.); vol. 89; 1; (2016); p. 103 – 111,9;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Related Products of 496-46-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 496-46-8, name is Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 9; PREPARATION OF A CUCURBITURIL TRIMER HAVING A RIGID ASSMEBLING UNIT; An exemplary pathway for preparing a cucurbituril trimer having a rigid assembling unit, according to the present invention, is presented in Figure 25. Coronene-1,2, 5,6, 9, 10-HEXANE (Figure 25, Compound 41), a derivative of coronene, is reacted with urea, so as to afford an assembling unit which includes three glycolurils units fused therein. The assembling coronene unit is then reacted with glycoluril, Compound 2, in a 1: 15 ratio, and with formaldehyde, in the presence of concentrated sulfuric acid, to thereby obtain the rigid derivatized cucurbituril trimer (Figure 25, Compound 42).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; TECHNION RESEARCH & DEVELOPMENT FOUNDATION LTD.; WO2005/23816; (2005); A2;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

496-46-8, name is Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, belongs to imidazoles-derivatives compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C4H6N4O2

EXAMPLE 2; AFFINITYPURIFICATION OFDIMETHYLCYCLOPENTANO-CB; Dimethylcyclopentano-CB (Figure 4, Compound 3) was synthesized according to the procedures described by Day et al. (J. Org. Chem. 2001, 66, 8094) and Isobe et al. (ORG. Lett. 2002, 4, 1287), by heating at 90 C for 24 hours, a 5 : 1 mixture of glycoluril (Compound 2) and dimethylcyclopentano-glycoluril (Figure 4, Compound 3), and formaldehyde in the presence of concentrated sulfuric acid (Figure 4), so as to give the desired cucurbituril product in 30 % yield. The water-soluble fraction (740 mg) of the crude, heterogeneous mixture (1.3 gram) was dissolved in neutral water (50 ml) and passed through a column loaded with the protonated aminated resin prepared as described above, at a flow rate of 0.5 ml/minute (of the heterogeneous mixture in water). The column was then washed sequentially with water, methanol, CH2C12, and again with methanol. Removal of the solvent from the combined eluent afforded a solid residue (510 mg). This residue was used for collecting a second harvest of CB [6] using the same column, as is detailed hereinbelow. A sample of the resin was dried under reduce pressure overnight and was analyzed by FTIR. The obtained spectrum, presented in Figure 13, indicated that the resin is indeed loaded with the CB [6]. The resin-bound CB [6] was released from the column by elution with a 1: 2 mixture of TRIETHYLAMINE-DMF (100 ml) at a flow rate of 2 ml/minute. The column was thereafter washed with water (200 ml), and the combined eluent was concentrated under reduced pressure. Methanol was then added and the precipitate was collected and dried. The resultant white powder (195 mg) was analyzed BY H NMR and ESI- MS and the analyses are presented in Figures 14 and 15, respectively. As is shown in Figures 14 and 15, the resin-bound CB [6], obtained as a powder upon elution from the column, contained mainly a mixture of Compound 4 (Figure 4) and Compound 1 (Figure 2), with a small amount of di (dimethylcyclopentano) -CB [6]. Regeneration of the column was performed by washing it with 10 % (v/v) trifluoroacetic acid in CH2C12. The regenerated column was used again to harvest additional amounts of CB [6] from the CB-depleted remnants obtained in the first harvest (510 mg). That residue was dissolved in neutral water and loaded on the column as described above. Unloading the column with triethylamine-DMF yielded a second crop of pure CB [6] (165 mg). The performance of the column over multiple cycles of affinity chromatography was evaluated by loading and unloading a sample of purified CB [6] (150 mg) four times. The sample was trapped and released quantitatively in all eight operations with no apparent loss of the column capacity.

The synthetic route of 496-46-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TECHNION RESEARCH & DEVELOPMENT FOUNDATION LTD.; WO2005/23816; (2005); A2;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 496-46-8, name is Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, A new synthetic method of this compound is introduced below., Application In Synthesis of Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione

After melting glycouryl (5.7 g, 40mmol) in 20 ml_ of sulfuric acid (9M), an aqueou s formaldehyde solution (7.0 mL, 91 mmol) was added. The resultant reaction mixture was stirred at 75 0C for 24 hours. The temperature was raised to 95-1000C, and the r eaction was further performed. 200 mL of water was quickly poured into the reaction mixture, and 1L of acetone was further added to obtain a precipitate. The precipitate was filtered under reduced pressure and washed with a 1 :4 mixed solution of water and acetone. The solid filtrate was dissolved in 200 mL of a 1 :1 mixed solution of water a nd acetone and filtered under reduced pressure to remove a precipitate (cucurbit[6]uril). 800 mL of acetone was added to the filtrate to precipitate a mixture of cucurbit[7 ]uril and cucurbit[5]uril. The precipitated mixture of cucurbit[7]uril and cucurbit[5]uril wa s dissolved in 40 mL of water, and 25 mL of methanol was added to precipitate only cue urbit[7]uril. The precipitated cucurbit[7]uril was filtered under reduced pressure and dri ed in a vacuum. The results of an analysis are as follows.1H NMR (500 MHz, D2O): delta = 5.56 (d, 14H), 5.35 (s, 14H), 4.11 (d, 14H).

The synthetic route of 496-46-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; POSTECH ACADEMY-INDUSTRY FOUNDATION; WO2007/46575; (2007); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

496-46-8, name is Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, belongs to imidazoles-derivatives compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C4H6N4O2

Synthesis of cucurbit[n]urils in hydrochloric acid using paraformaldehyde Unsubstituted glycoluril (20 g) and hydrochloric acid (37 % w/v, 30 mL) were placed in a reaction flask and heated to 90C. Paraformaldehyde (8.87 g) was added in portion-wise and the reaction mixture was then heated to 100 C (internal) for 18 hours. The reaction mixture was cooled and added to methanol (150 mL) to produce a beige powder which was analysed by1H NMR.Approximate Yields by1H NMR (% of recovered product) cucurbit[5]uril 8%, cucurbit[6]uril 44%, cucurbit[7]uril 28%, cucurbit[8]uril 18%, cucurbit[9]uril 0%, cucurbit[10]uril 0% cucurbit[11]uril 0%.Residual formaldehyde by HPLC method was 682 ppm.

The synthetic route of 496-46-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AQDOT LIMITED; COULSTON, Roger; DIEC, David; NOGUEIRA, Guilherme; GERARDUS DE ROOIJ, Johannes; (23 pag.)WO2018/115822; (2018); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Related Products of 496-46-8, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 496-46-8, name is Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of the diether (compound 2.5) of dimethylglycoluril (1 g, 3.9 mmol), glycoluril (1. 1 g, 7.75 mmol) and LICL (250 mg) were ground together to give a fine powder. To this mixture was added 8 M HCL (10 mL) and the mixture stirred for 1 hr at ambient temperature, after which time all the solid material had dissolved. The mixture was then heat at 50C for 12 to 24 hr. After cooling the solvent was evacuated in vacuo. Re- crystallisation from combinations of methanol and dilute acid solutions gave the trimer (compound 2.4) 1.2 g as a pure compound.

The chemical industry reduces the impact on the environment during synthesis Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione. I believe this compound will play a more active role in future production and life.

Reference:
Patent; UNISEARCH LIMITED; WO2005/26168; (2005); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem