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Reaction in solution phase between commercial rhodanine and benzyl bromide afforded a ratio of 4:1 for sulfur/nitrogen alkylation, see Ref. 8.
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44
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34447555458
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note
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® 402 Prolabo microwave reactor. The stirred mixture was irradiated (after a ramp of 4 min from 20 to 80 °C) at 80 °C (Power level: 30%, 90 W) with appropriate reaction time (from 20 to 60 min). After microwave dielectric heating, the crude reaction mixture was allowed to cool down at room temperature and ethanol (20 mL) was added in the cylindrical quartz reactor. The resulting insoluble product 6 was filtered and dried under high vacuum for 2 h.
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45
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CAUTION: Owing to elimination of hydrogen sulfide during the sulfur/nitrogen displacement reaction, the experiments in the microwave reactor were realized under ventilated extractor hood.
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-
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46
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34447564706
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note
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+ requires 318.0674).
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