Synthetic Route of 101335-11-9, A common heterocyclic compound, 101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, molecular formula is C6H3ClFI, 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.
Intermediate XI A solution of isopropyl magnesium chloride (100 mL, 2.0M in Ethyl Ether) was added to a solution of 2-chloro-4-fluoro-1-iodobenzene (25 g, 97.5 mmol) in 300 mL THF chilled in an ice bath. The solution was then stirred at RT overnight. The solution was chilled in a CO2/acetone bath and trimethyl borate was added (23 mL, 200 mmol). The solution was warmed to RT and stirred for 6 h. The suspension was partitioned between water and ethyl ether (emulsion). The phases were separated and the organic phase concentrated. The residue was treated with 200 mL 2N HCl and stirred overnight. The suspension was then extracted with ethyl ether (2*) and the combined organics washed with brine, dried over MgSO4, filtered and concentrated to give 13.3 g solid. The crude solid was suspended in hexanes, filtered and washed 2* (hexanes) to give 2-chloro-4-fluoro-phenylboronic acid. LC 1: 1.65 min.
The synthetic route of 101335-11-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Doherty, James B.; Stelmach, John E.; Chen, Meng-Hsin; Liu, Luping; Hunt, Julianne A.; Ruzck, Rowena D.; Goulet, Joung L.; Wisnoski, David D.; Natarajan, Swaminathan Ravi; Rupprecht, Kathleen M.; Bao, Jianming; Miao, Shouwu; Hong, Xingfang; Sinclair, Peter J.; Kallashi, Florida; US2003/92712; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com