Synthetic Route of 36556-52-2, These common heterocyclic compound, 36556-52-2, name is 2,3-Dichloro-4-fluoroaniline, 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.
To a vial containing 2,3-dichloro-4-fluoroaniline (307.4 mg, 1.7 mmol) in 2 mL toluene was added 4M HCl in 1,4-dioxane (0.43 mL, 1.7 mmol) followed by phosgene (20% in toluene; 3.6 mL, 6.8 mmol). Precipitate formed upon HCl addition. The vial was capped and heated to 100 C. After 30 min, all the solids had disappeared. After 6.5 h, the solvent was removed under vacuum. Material was re-dissolved in toluene, and solvent was again removed under vacuum to eliminate any remaining phosgene. The resulting material was a brown oil that crystallized upon standing and was used without further purification. A capped vial containing 7 (108.8 mg, 0.55 mmol) and 2,3-dichloro-1-fluoro-4-isocyanatobenzene from above (~0.55 mmol) was heated to 70 C. After 2 days, solvent was removed under vacuum. The oil residue was treated with DCM, producing a precipitate. The resulting mixture was left to stand at room temperature for >30 min. The solids were filtered, washed with minimal amount of DCM and dried under vacuum to give119.1 mg (54%) of 8k as an off-white solid. The material was used without further purification.
The synthetic route of 36556-52-2 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Moffett, Kristofer; Konteatis, Zenon; Nguyen, Duyan; Shetty, Rupa; Ludington, Jennifer; Fujimoto, Ted; Lee, Kyoung-Jin; Chai, Xiaomei; Namboodiri, Haridasan; Karpusas, Michael; Dorsey, Bruce; Guarnieri, Frank; Bukhtiyarova, Marina; Springman, Eric; Michelotti, Enrique; Bioorganic and Medicinal Chemistry Letters; vol. 21; 23; (2011); p. 7155 – 7165;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics