Reference of 30169-25-6, 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. 30169-25-6 name is 3,6-Bis(3,5-dimethyl-1H-pyrazol-1-yl)-1,2,4,5-tetrazine, 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.
To a solution of 3,6-bis(3,5-dimethylpyrazolyl)-1,2,4,5-tetrazine (2.72 g, 10.0 mmol) in MeCN (10 mL) was added DNAZ.HCl (1.83 g, 10.0 mmol) and triethylamine (1.11 g, 11 mmol). The resulting solution was stirred for 1 hour until the color had changed to a uniform orange-red color. Diethyl ether (20 mL) was added and the precipitate was collected via filtration. The precipitate was washed with water (3×10 mL) and diethyl ether (2×10 mL). Recrystallization of the crude material from MeCN led to isolation of DMPTzDNAZ (2, 2.50 g, 78%) as orange-red crystals. Anal. Calcd for C10H11N9O4: C, 37.39%; H, 3.45%; N, 39.24%. Found: C, 37.73%; H, 3.42%; N, 38.89%. 1HNMR (400 mHz, d6-DMSO) delta 2.24 (s, 3H, CH3), 2.46 (s, 3H, CH3), 5.28 (s, 4H, DNAZ), 6.26 (s, 1H, pyr). 13CNMR (400 mHz, d6-DMSO) delta 12.67 (CH3), 13.37 (CH3), 59.71 (DNAZ), 107.95 (DNAZ), 109.50 (pyr), 141.88 (pyr), 151.10 (pyr), 157.71 (tz), (Tz), 162.58 (tz).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,6-Bis(3,5-dimethyl-1H-pyrazol-1-yl)-1,2,4,5-tetrazine, and friends who are interested can also refer to it.
Reference:
Patent; Los Alamos National Security, LLC; Chavez, David E.; Hanson, Susan Kloek; Scharff, Robert Jason; Veauthier, Jacqueline Marie; Myers, Thomas Winfield; (40 pag.)US9902748; (2018); B2;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics