Category: 17464-88-9

Electric Literature of 17464-88-9, A common heterocyclic compound, 17464-88-9, name is 1,3,4,6-Tetrakis(methoxymethyl)tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, molecular formula is C12H22N4O6, 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.

The Amberlyst 15 resin was dried in an oven to 60% of the original weight.3 g of tetramethoxymethylglycoluril was added to a 250 ml three-necked flask, 6 g of Amberlyst15 resin after drying, and 70 g of PGME were added, and the temperature was raised to 60 C. The reaction was stirred at -0.07 MPa for 17 hours while the produced methanol was distilled off.The reaction was filtered through a Buchner funnel and the filter was washed twice with PGME to recover the resin.The filtrate and the washing solution were combined and the solvent PGME was distilled off under reduced pressure to obtain 5.19 g of 1,3,4,6-tetrakis (1′-methyl-2′-methoxy) ethoxymethylglycol, 99.8%

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Shanxi Medical University; Zhao Zhengbao; Liang Rui; Zhang Jiancheng; Liu Ruiling; Wei Xiao; Li Feifei; (7 pag.)CN105085532; (2017); B;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Synthetic Route of 17464-88-9, 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. 17464-88-9 name is 1,3,4,6-Tetrakis(methoxymethyl)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.

60 g (0.188 mol) of tetramethoxymethylglycoluril (product name: POWDERLINK [registered trademark] 1174 commercially available from Japan Cytec Industries, hereinafter abbreviated as PL-LI in this specification), 1,200 g of propylene glycol monomethyl ether (hereinafter abbreviated as PGME in this specification), and 120 g of a washed ion-exchange resin for a catalyst (product name: AMBERLYST [registered trademark] 15JWET, commercially available from Dow Chemical Company, hereinafter abbreviated as 15JWET in this specification) were put into a 2,000 mL flask, and the mixture was stirred and dissolved at 25¡ã C. and then heated and stirred under a reduced pressure (80 Torr to 100 Torr) at 60¡ã C. for 7 hours. Then, the pressure inside the flask was recovered and cooling was performed to 25¡ã C., and then 15JWET was filtered off to obtain a desired compound (hereinafter abbreviated as PGME-PL in this specification). The obtained compound was identified by 1H NMR. As a result, it was confirmed that a peak (31.9 ppm) of a methoxy group of PL-LI disappeared and about 4 molecules of PGME were introduced into one molecule of PL-LI, and the glycoluril derivative of Formula (1A-1) (hereinafter abbreviated as PGME-PL in this specification) was obtained. [1.0 to 1.1 ppm (3H, ?CH3), 3.2 to 3.3 ppm (20H, ?OCH3 and ?CH2O?), 3.6 to 3.8 ppm (4H, ?OCH<)] At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3,4,6-Tetrakis(methoxymethyl)tetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, and friends who are interested can also refer to it. Reference:
Patent; NISSAN CHEMICAL CORPORATION; SAKAIDA, Yasushi; TAKASE, Kenji; KISHIOKA, Takahiro; SAKAMOTO, Rikimaru; (14 pag.)US2019/163063; (2019); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem