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