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ChemicalBook CAS DataBase List 2-Chloro-3-fluoronitrobenzene
21397-07-9

2-Chloro-3-fluoronitrobenzene synthesis

6synthesis methods
1-Fluoro-3-nitrobenzene

402-67-5

2-Chloro-3-fluoronitrobenzene

21397-07-9

General procedure for the synthesis of 2-chloro-3-fluoronitrobenzene from 3-fluoronitrobenzene: To a solution of 3-fluoronitrobenzene (2 g, 14.2 mmol) in tetrahydrofuran (THF, 30 mL) was slowly added a solution of N-chlorosuccinimide (5.69 g, 42.6 mmol) in THF (20 mL) at -78 °C. Subsequently, NaHMDS (28.4 mL, 28.4 mmol) in a 1 M solution of THF was added dropwise while ensuring that the internal temperature of the reaction system was maintained below -75 °C. The reaction mixture was stirred continuously at -78 °C for 30 min. Upon completion of the reaction, the mixture was partitioned between 5% hydrochloric acid and ethyl acetate. The organic layers were combined, dried with anhydrous magnesium sulfate (MgSO4), filtered and the solvent evaporated. The resulting solid was purified by silica gel column chromatography with the eluent being a hexane solution of 20% ethyl acetate, resulting in the target product 2-chloro-3-fluoronitrobenzene (231 mg, 9.2% yield). The structure of the product was confirmed by EI-MS, m/z 176.5 (M+).

-

Yield:21397-07-9 79.8%

Reaction Conditions:

with hexachloroethane;lithium tert-butoxide in N,N-dimethyl-formamide at 60; for 4 h;Inert atmosphere;regioselective reaction;

Steps:

Synthetic procedure of compound 6

A solution of 1-fluoro-3-nitrobenzene (1.41g, 10mmol), t-BuOLi (2.00g, 25mmol) and C2Cl6 (4.73g, 20 mmol) in 15ml dry DMF was stirred for 4h at 60°C under N2 atmosphere. Ethyl acetate was added and the resulting organic solution was washed by 1M HCl, saturated NaHCO3 and brine successively. The solvent was removed under reduced pressure and the residue was purified on column chromatography (eluted by 0.5% ethyl acetate in petroleum ether) to obtain 6 as a colorless oil. Yield: 79.8%, 1H NMR (400 MHz, CDCl3) δ 7.77-7.69 (m, 1H, Ph-H), 7.48-7.41 (m, 2H, Ph-H).

References:

Wei, Wei;Zhou, Shaa;Cheng, Dandan;Li, Yuxin;Liu, Jingbo;Xie, Yongtao;Li, Yonghong;Li, Zhengming [Bioorganic and Medicinal Chemistry Letters,2017,vol. 27,# 15,p. 3365 - 3369] Location in patent:supporting information

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