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ChemicalBook CAS DataBase List 2-Chloro-6-fluorophenylisothiocyanate
899806-25-8

2-Chloro-6-fluorophenylisothiocyanate synthesis

3synthesis methods
-

Yield:899806-25-8 17%

Reaction Conditions:

in tetrahydrofuran at 20; for 60 h;

Steps:

5.18

[00311] Synthesis of 6-chloro-2-fluorobenzeneisothiocyanate; [00312] A solution of 2-chloro-6-fluoroaniline (767 mg, 5.29 mmol) in tetrahydrofuran (5 ml) was added drop wise with stirring to a solution of di-2-pyridyl thionocarbonate (2.46 g, 10.58 mmol) in tetrahydrofuran (7 ml) at room temperature. The reaction mixture was stirred for 60 hours at room temperature and then the solvent was evaporated. The resulting residue was purified by chromatography on a normal phase silica gel column with pentane. Fractions containing clean product were combined and the solvent evaporated to give the title compound (167 mg, 17%): 1H NMR (400 MHz, CDCl3) δ 7.19- 7.23 (m, IH), 7.12-7.19 (m, IH), 7.04-7.10 (m, IH).

References:

WO2006/76595,2006,A1 Location in patent:Page/Page column 153