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