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0011387030
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note
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11. Typical experimental procedure: To a degassed, refluxing solution of xanthate 5 in 1,2-dichloroethane (0.1 mmole / ml) is added dilauoyl peroxide in 5 mole% portions every hour until consumption of the starting material (1-1.5 mole-equivalents are usually needed). Alternatively, the higher boiling chlorobenzene can be used and a 0.1M peroxide added over 0.5-1 hour. In both cases, the reaction is regularly monitored for the disappearance of the starting material by thin-layer chromatography. Upon completion, the solvent is removed under partial vacuum and the residue purified by chromatography.
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29
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Ando, W., Ed; J. Wiley & Sons: Chichester; Chap. 7
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Kujimori, K.1
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