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. name: 5-Amino-1,3-dimethylpyrazole
A mixture of 5-amino-1,3-dimethyl-pyrazol (1.87 g, 16.8 mmol), 2,4-dichlorobenzaldehyde (2.95 g, 16.8 mmol, Fluorochem), and 2-mercapto-2-methylpropanoic acid (2.5 g, 20.8 mmol) was heated, in a microwave for about 60 min, at about 100 C. Subsequently, the reaction mixture was sealed and heated, for about 24 h, at about 150 C. After cooling to rt, THF (300 ml) was added, followed by EDC.HCl (4.25 g, 22 mmol) and DMAP (4-dimethylamino-pyridine, 0.2 g, 1.64 mmol). Subsequently, the reaction mixture was stirred for about 24 h, at rt. NaOH (2 M aqueous, 10 mL) and ethyl acetate (200 mL) were added. The layers were separated and the aqueous layer was extracted with ethyl acetate (50 mL). The combined organic layers were washed with water (2×50 mL), dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by column chromatography (SiO2, diethyl ether, followed by ethyl acetate) to afford 4-(2,4-dichlorophenyl)-1,3,6,6-tetramethyl-4,8-dihydropyrazolo[3,4-e][1,4]thiazepin-7-one (3.11 g, 8.4 mmol, 50%) as white solid: 1H-NMR (CDCl3, Bruker 400 MHz) delta 1.51 (3H, s); 1.64 (3H, s); 1.67 (3H, s); 3.78 (3H, s); 5.77 (1H, s); 7.17 (1H, dd, J=8.4, 2.0 Hz); 7.28 (1H, d, J=8.4 Hz); 7.41 (1H, d, J=2.0 Hz); H, m); 8.43 (1H, bs).
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.