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33646650313
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note
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3Ni]
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50
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33646666413
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note
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int = 0.0449). R = 0.0341, Rw = 0.0807 (on 1700 observed reflections [I > 1.00r(I)] and 133 variable parameters).
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56
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33646643199
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note
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General procedure for the methylthiolation of iodobenzene. Under an atmosphere of nitrogen, a solution of 4.9 mmol of iodobenzene, 2.45 mmol of methyl disulfide, 3.0 mg of catalyst 5 (0.0057 mmol) and 202 mg (0.924 mmol) of diethylene glycol di-n-butylether (internal standard) in 3.0 mL of DMF was introduced into a Schlenk tube containing a magnetic stir bar and charged with 4.9 mmol of zinc dust. The tube was sealed and fully immersed in a 110°C silicon oil bath. After 4 h, the reaction mixture was cooled to room temperature and, the organic phase analyzed by gas chromatography (GC-MS).
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