Extracurricular laboratory: Synthetic route of 714273-83-3

The synthetic route of 714273-83-3 has been constantly updated, and we look forward to future research findings.

Reference of 714273-83-3, A common heterocyclic compound, 714273-83-3, name is 5-(tert-Butyl)-1H-imidazole-4-carbaldehyde, molecular formula is C8H12N2O, 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.

In 5000 ml dry three-mouth flask was added magnesium chips (14.4g, 0.60 mol) and dry tetrahydrofuran (1L). Drop 1ml 1,2-dibromoethane and initiate the reaction. Then slowly add dropwise bromoacetaldehyde ethylene acetal (100g, 0.60 mol) in tetrahydrofuran solution (500 ml). After adding dropwise, stir for two hours until magnesium chips disappear. Then 5-tert-butyl-1H-imidazole-4-carbaldehyde (30g, 0.20 mol) in tetrahydrofuran solution (500 ml) was slowly added dropwise to the above solution. Stir overnight. Then use concentrated hydrochloric acid to adjust to acidic (pH=1), and heated to 60 C and stir for 30 minutes. Steaming and remove the tetrahydrofuran, adding the ethyl acetate extraction. The organic phase and water washing twice, a saturated salt water washing, final drying with anhydrous sodium sulfate, concentrated. The crude product is purified by column chromatography (petroleum ether/ethyl acetate of the volume ratio: 2/1) to obtain a yellow solid (17.8g, yield: 50%).

The synthetic route of 714273-83-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shenzhen Haiwang Pharmaceutical Technology Research Institute Co., Ltd.; Tang, Tian; Peng, Jianghua; Wu, Jing; Feng, Yidong; Yang, Jingan; She, Qin; Feng, Hanlin; (28 pag.)CN106565685; (2017); A;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem