Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 10570-40-8, name is 4-Methyl-4H-1,2,4-triazole, A new synthetic method of this compound is introduced below., category: Triazoles
4.2 1-(4-Methyl-4H-1,2,4-triazol-3-yl)octan-1-ol To a solution of 4-methyl-1,2,4-triazole (681 mg, 7.78 mmol), TMEDA (0.40 ml) in dry THF (10 ml) and at -60 C, 2.69 M n-BuLi solution (2.9 ml, 7.80 mmol) was added drop wise. After stirring at -60 C for 30 min, 10 ml of dry THF solution of octanol (1.30 mL, 8.33 mmol) was added and the mixture was stirred for additional 4 h at -60 C to -30 C. Then H2O was added and the mixture was extracted three times with ethyl acetate. The organic layer was washed with saturated brine and dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (1-5% methanol/chloroform) as a colorless solid (1.13 g, 69%): Mp. 63-65 C; 1H NMR (500 MHz, CDCl3) delta 0.87 (3H, t, J = 6.6 Hz), 1.30-1.26 (9H, m), 1.46 (1H, q, J = 5.2 Hz), 1.93-1.84 (2H, m), 3.50 (1H, br s), 3.93 (3H, s), 4.82 (1H, q, J = 6.3 Hz), 7.76 (1H, s); 1H NMR (300 MHz, DMSO) delta 0.88 (3H, t, J = 6.9 Hz), 1.26-1.49 (14H, m), 1.87-1.93 (2H, m), 2.70 (1H, d, J = 7.5 Hz) 3.92 (3H, s), 4.84 (1H, q, J = 6.9 Hz), 7.79 (1H, s); 13C NMR (126 MHz) delta 14.1, 22.7, 25.2, 29.5, 31.9, 33.7, 35.4, 39.8, 64,2, 143.6, 155.0; HRMS (ESI) m/z calcd for C11H21N3NaO (M + Na)+ 234.1582, found. 234.1573.
The synthetic route of 10570-40-8 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Suzuki, Yumiko; Iwata, Naoto; Dobashi, Kohei; Takashima, Ryo; Arulmozhiraja, Sundaram; Ishitsubo, Erika; Matsuo, Naoya; Tokiwa, Hiroaki; Tetrahedron; vol. 74; 3; (2018); p. 392 – 400;,
1,2,3-Triazole – Wikipedia,
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