These common heterocyclic compound, 16778-70-4, name is 1-Ethyl-1,2,4-triazole, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. HPLC of Formula: C4H7N3
Intermediate 72; l-(2-Ethyl-2H-ri.2.41triazol-3-yl)-ethanone; n-Butyl lithium (424 ml, 1.6M solution in THF, 0.679 moles) was added dropwise to a solution of l-ethyl-lH-l,2,4-triazole (55 g, 0.566 moles) in THF (400 ml) at 0 C. After stirring for 1 hr at 0 C, N,N-dimethylacetamide (63 ml, 0.679 moles) was added to the reaction mixture and the stirring was continued for 1 hr. The progress of the reaction was monitored by TLC. The reaction mixture was quenched with sat. ammonium chloride solution and extracted with DCM. The combined organic layers were dried over sodium sulfate and concentrated. The crude material was purified by column chromatography (100% hexane followed by gradient elution to 10% ethyl acetate in hexane). Product (70 g) was obtained as light yellowish liquid. (Note : Since the product is volatile, it has to be distilled at less than 400 C) NMR (400 MHz, CDC13, delta): 1.42 (t, 3H), 2.69 (s, 3H), 4.58 (q, 4H), 7.90 (s, IH). MS (ES) (M+H)+: 140 for C6H9N3O.
The synthetic route of 1-Ethyl-1,2,4-triazole has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; PEER MOHAMED, Shahul, Hameed; WATERSON, David; WO2010/67125; (2010); A1;,
1,2,3-Triazole – Wikipedia,
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