Continuously updated synthesis method about 3524-32-1

According to the analysis of related databases, 3524-32-1, the application of this compound in the production field has become more and more popular.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 3524-32-1 as follows. Quality Control of 5-Amino-1,3-dimethylpyrazole

Step 1 N-(2,5-Dimethyl-2H-pyrazol-3-yl)-2,2-dimethyl-propionamide To 15.0 g (131 mmol) N-(2,5-dimethyl-2H-pyrazol-3-yl)-amine in 150 mL pyridine at 0 C. was added 19.3 mL (18.9 g, 158 mmol) of pivaloyl chloride. After stirring at 23 C. for 3.5 hours, the reaction solvent was evaporated, and the residue was evaporated with 2*200 mL toluene. The remaining solid was dissolved in 500 mL EtOAc/200 mL H2O and extracted. The aqueous layer was extracted with 2*100 mL EtOAc, and the combined organics were washed with 1*200 mL brine, dried over MgSO4, filtered and evaporated to an orange solid. Recrystallization from hot hexanes/EtOAc gave 24.45 g (125 mmol, a 96% yield) of the title compound as an off-white, crystalline solid: mp: 86-88 C.; 1H NMR (300 MHz, CDCl3): delta 1.32 (s, 9H), 2.22 (s, 3H), 3.63 (s, 3H), 5.98 (s, 1H), 7.12 (brs, 1H); IR (KBr, cm-1): 3316s, 3274s, 2967m, 2935m, 1673s, 1655m, 1570s, 1514m, 1492m, 1457m; MS (ES) m/z (relative intensity): (196, M+, 100). Anal. Calcd. for C10H17N3O: C, 61.51; H, 8.77; N, 21.52. Found: C, 61.33; H, 8.80; N, 21.23.

According to the analysis of related databases, 3524-32-1, the application of this compound in the production field has become more and more popular.