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ChemicalBook CAS DataBase List CUCURBIT(7)URIL
259886-50-5

CUCURBIT(7)URIL synthesis

7synthesis methods
-

Yield:259886-50-5 24%

Reaction Conditions:

with sulfuric acid at 75 - 100; for 36 h;

Steps:


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): δ5.76(1H, d, H-1 of CB),4.21(1H, d, H-2 of CB), 5.49(1H, s, H-3 of CB).

References:

Gao, Chuanzhu;Jia, Chunyan;Li, Yamin;Liao, Xiali;Yang, Bo;Zhang, Xinzhong;Zhong, Yunshuang [Journal of Inclusion Phenomena and Macrocyclic Chemistry,2020]

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