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6 (0.1 mL) was added for lock purpose.
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0011447830
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3SnC≡CH is volatile enough to be lost under these condition, thus obtaining wrong information on completion of step 1.
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42
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Formation of insoluble material might be related to the formation of insoluble higher-order polymers.
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2,5-Bis[(tributyltin)ethynyl]thiophene (4) is a high-boiling oily material whose purification is very difficult. Attempts of performing vacuum distillation lead to thermal decomposition; chromatographic separation partially cleaves tributyltin groups.
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