Category: 496-46-8

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., Formula: C4H6N4O2

In a 1,000-liter reactor was charged 320 kg of water, Heated to reflux, 71 kg of glycoluril and 58 kg of 50% glyoxal were successively added, Stirring to clear, In the refluxing state, 500 L of a sodium hydroxide solution (8 mol / l) was rapidly added dropwise, After completion of the dropwise addition, The refluxing reaction was continued for 8 hours. Close the heating,When the temperature naturally cool to room temperature,45 kg of chlorine gas was introduced into the reaction system,After completion of the reaction,Concentrated hydrochloric acid was added to adjust the pH to 1,Stirring was reduced to room temperature,After 2 hours,Obtain crude orotic acid.In the 2000-liter reactor, the crude orotate was added and 600 kg of water was added. After boiling, add the concentrated ammonia to dissolve, then add 5 mol / L sulfuric acid to adjust the pH to weak acidity, add activated carbon to boil for 30 minutes, filter it hot, adjust the pH to 1 with concentrated sulfuric acid, Dry, get whey acid finished 25.7 kg, yield 33%, purity 99.9%.

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

Reference:
Patent; Chengdu Baishixing Science and Technology Industry Co., Ltd.; Shi, Changqing; (6 pag.)CN106187918; (2016); A;,
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. Quality Control of Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione

Synthesis of cucurbit[n]urils in methanesulphonic acid (MSA) using paraformaldehydeUnsubstituted glycoluril (20 g) and methanesulphonic acid (neat, 82 mL) were placed in a reaction flask and heated to 90 C. Paraformaldehyde (8.45 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 (410 ml) to produce a brown powder which was analysed by1H NMR.Approximate Yields by1H NMR (% of recovered product) cucurbit[5]uril 0%, cucurbit[6]uril 63%, cucurbit[7]uril 35%, cucurbit[8]uril 0%, cucurbit[9]uril 0%, cucurbit[10]uril 0% cucurbit[11]uril 0%.Residual formaldehyde by HPLC method was 1621 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

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., Recommanded Product: Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione

The tetrol derivative (compound 2.6) of 3a, 6a- cyclopentanoglycoluril (1 g, 3.3 mmol) was added to a solution of unsubstituted glycoluril (937 mg, 6.6 mmol) in conc. HCL (2 mL) and the mixture stirred at room temperature for 30 min. The homogeneous mixture was poured into MEOH (10 mL) and the precipitate collected and dried to give predominantly the trimer.

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

Electric Literature of 496-46-8, A common heterocyclic compound, 496-46-8, name is Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, molecular formula is C4H6N4O2, 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.

CB[7] was synthesized according to the published procedures[35, 36]. Reaction of glycoluril with formaldehyde in 9 M sulfuric acid at ~ 75 C for 24 h and then at ~ 100 C for12 h yielded a mixture of CB[n]. After the reaction, the mixture was poured into water, acetone was added to produce precipitate. The precipitate was separated by decantation,washed with water/acetone, and filtered. From the acetone/water soluble portion, CB[7] were isolated by fractional crystallization/precipitation and further purified by recrystallizatio.The prepared CB[7] has a purity of 99% and ayield of 24%. Anal. Calc. for C42H42N28O14(M = 1162.96 g/mol): C: 43.34%, H: 3.61%, N: 33.71%, O: 19.26%. Found:C: 42.62%, H: 3.47%, N: 34.47%, O: 18.69%. 1H-NMR(400 MHz, D2O,TMS, ppm): delta5.76(1H, d, H-1 of CB),4.21(1H, d, H-2 of CB), 5.49(1H, s, H-3 of CB).

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

Reference:
Article; Gao, Chuanzhu; Jia, Chunyan; Li, Yamin; Liao, Xiali; Yang, Bo; Zhang, Xinzhong; Zhong, Yunshuang; Journal of Inclusion Phenomena and Macrocyclic Chemistry; (2020);,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Reference 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.

Example 2: Synthesis of cucurbituril homologues; [27] 3 g of paraformaldehyde was added to 5.68g of glycolurils of formula 9 and 20 mL of a 9M sulfuric acid was added thereto. Then, a 800W microwave was irradiated to the reaction mixture for 45 seconds. [28] The reaction solution was recrystallized with acetone and methanol to thereby synthesize and separate four cucurbituril homologues, CB[5], CB[6], CB[7], and CB[8 ], as represented by formula 1 where X is 0, Rand R are H, and n is 5,6, 7, and 8, respectively. The yields of CB[5], CB[6], CB[7], and CB[8] were 15%, 45%, 20%, and 15%, respectively. [29] CB [5]:¹ H (500 MHz, D 2O/CF CO DID SO 4 (1:1:0.15)): No. 4.43 (d, J = 15.5 Hz, 10H), 5.65 (s, 10H), 5.85 (d, J =15.5 Hz, lOH). [30] CB [6]:¹ H (500 MHz, D 2 O/CF 3CO2 DID 2 SO 4 (1: 1:0.15)): No. 4.35 (d, J = 15.5 Hz, 12H), 5.61 (s, 12H), 5.69 (d, J =15.5 Hz, 12H). [31] CB [7]:¹ H (500 MHz, D 2 O/CF 3CO2 DID 2 SO 4 (1: 1:0.15)): No. 4.29 (d, J = 15.5 Hz, 14H), 5.60 (s, 14H), 5.91 (d, J =15.5 Hz, 14H). [32] CB [8]:¹ H (500 MHz, D 2 O/CF 3CO2 DID 2 SO 4 (1: 1:0.15)): No. 4.28 (d, J = 15.5 Hz, 16H), 5.60 (s, 16H), 5.93 (d, J =15.5 Hz, 16H).

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; POSTECH ACADEMY-INDUSTRY FOUNDATION; WO2005/103053; (2005); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Synthetic Route of 496-46-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 496-46-8 name is Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

10 mol of glycoluril (Sigma-Aldrich) was diluted in propylene glycol monomethyl ether acetate. While the solution was maintained at 50 C., a solution obtained by diluting 40 mol of glycidyl acrylate (Sigma-Aldrich) in the same solvent was slowly added thereto to allow the mixture to react. The obtained solution was separated through a column, and then the solvent was removed by using vacuum distillation, thereby obtaining a compound represented by [Formula 11]. The procedure was repeated to prepare a sufficient amount of the compound of [Formula 11]. (0093) (0094) The structure was confirmed through 1H-NMR. 5.80, 6.05, 6.43 (-CH=CH2), 3.43, 4.28, 4.43, 4.44 (aliphatic H), 2.0 (-OH)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, and friends who are interested can also refer to it.

Reference:
Patent; LG Chem, Ltd.; Lee, Keon Woo; Kwak, Sang Kyu; Lee, Changsoon; Kim, Hyehyeon; Kim, Saehee; US8828644; (2014); B2;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Synthetic Route 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.

Into a suitable reaction vessel equipped with a stirrer, thermometer and reflux condenser, there was introduced 688 parts (10 mol) of aqueous formaldehyde (44%), and the pH was adjusted to 8.7 with 22 parts of 0.5 N NaOH solution. To this solution, there was added 284 parts (2 mol) of acetylene carbamide at 40 C. During the resulting reaction, the temperature was allowed to rise up to 55 C. At this stage, most of the acetylene carbamide entered into solution. After about 15 minutes, the pH was adjusted to 8.0 with five parts of 0.5 N NaOH. A clear, pale yellow colored solution was obtained. The clear solution was distilled at 50 C, under reduced pressure, to remove water until the reaction vessel content was about 640 parts. The resulting syrup in the vessel was poured into 800 parts of methanol. The resulting white crystalline precipitate was filtered and dried. The total yield of the tetramethylol acetylene carbamide was 483 parts (92%) and had a melting point of 132 – 136 C.

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; ROTAM AGROCHEM INTERNATIONAL COMPANY LIMITED; BRISTOW, James Timothy; WO2014/166347; (2014); 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.

(0044) The original patent for structure 1, FIG. 1 was granted in 1984 to J. Boileau. His synthetic methodology for successfully achieving 1 was the direct nitration of glycoluril using a mixture of N2O5 and 100% HNO3. The yields on his process are claimed to be greater than 85%. It has since been discovered it is possible to successfully synthesize structure 1 using a mixture of acetic anhydride and 100% HNO3 in similar yields without necessitating the making N2O5 directly. Both of these methods yield structure 1 that is highly sensitive to impact and friction (approximately twice more sensitive on both accounts than standard military explosives RDX and HMX) making handling of the material from these processes inherently more dangerous.

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; U.S. Army Research Laboratory ATTN: RDRL-LOC-I; Sherrill, William Matthew; Banning, Joseph Erik; (7 pag.)US2016/90388; (2016); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Reference of 496-46-8, A common heterocyclic compound, 496-46-8, name is Tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, molecular formula is C4H6N4O2, 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.

3a-isopropylglycoluril dimer diether (compound 2.3) (1 g, 2.5 mmol) and unsubstituted glycoluril (720 mg, 5.0 mmol) were mixed in 7M hydrochloric acid (12 mL). The mixture was stirred at room temperature for 1 hr. The mixture was heated to 100C for 2-3 hr. Evaporation of the acid in vacuo gave the a, P, 5, G-TETRAISOPROPYLCUCURBIT [4,2] uril as the major product.

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

Reference:
Patent; UNISEARCH LIMITED; WO2005/26168; (2005); 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. category: imidazoles-derivatives

Preparation of a cucurbituril trimer (Figure 23, Compound 38) :; As is exemplified in Figure 23, an exemplary pathway for forming a cucurbituril trimer involves a disubstituted cucurbituril derived from benzil. Such a pathway generally includes preparation of a benzil-derived glycoluril, as described hereinabove, a formation OF A DERIVATIZED CB monomer, and a trimerization step. As a starting material, a benzil-derived glycoluril (Figure 23, Compound 35) is prepared by reacting a para-substituted benzil with urea in a 1: 2 ratio in benzene and trifluoroacetic acid, according to the exemplary syntheses are presented hereinabove. In one non-limiting example, one of the para-substituents on the benzil is a carboxyl group and the second is hydrogen (Figure 23, Compound 34). Compound 35, is reacted with glycoluril, Compound 2, in a 1: 5 ratio, and with formaldehyde, in the presence of concentrated sulfuric acid, to thereby form the derivatized cucurbituril biphenyl-CB [6] (Figure 23, Compound 36). Compound 36 is reacted with 1,3, 5-benzenetriamine (BTA) in a 3: 1 ratio so as to form three amide bonds between each of the carboxyl groups on the derivatized CB [6] and an amine on the BTA, and thus form a cucurbituril trimer having a BTA as the assembling unit (Figure 23, Compound 38).

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