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The authors rely heavily on 1HNMR characterization. For quantification this is not always appropriate. End groups are small and often shielded by larger resonances.

PEO-TEMPO and PCL-TEMPO should therefore also be analyzed by MALDI MS In fig 6 and more particularly Fig 9, a clear shoulder and low molecular weight fraction are visible in the trace of the triblock copolymers. This raises doubts over the complete formation and purity of the triblock copolymer.  Most appropriate would be to analyze the samples with 2D chromatography. Another option would be to treat the samples with scavenger resin (azide and alkyne functional Merrifield resin for removal of unreacted alkynes and azides.)



What is the yield of the triblock copolymers after work up?



The triblock coupling efficiency as is calculated should be reformulated to show the ratio between the different blocks. This gives much more valuable information, because it can show the efficiency  of both coupling procedures. The calculation procedure can be shifted to the suppl. info.



Why is the reaction performed at 90¡ãC? This one pot procedure could in principle also be performed at lower temperatures, which would yield another benefit toward other procedures. This experiment is strongly recommended. If it has already been investigated, then a comment on temperature effects should be included.



For the one-pot procedure one equivalent of CuBr is used, which is in principle fully used by ATRNC. This could lead to problems with the click chemistry coupling. The authors should comment about this (is click chemistry much faster than ATRNC?, have they investigated different ratios of CuBr?).

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lovehappy2008

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1 The authors rely heavily on 1HNMR characterization. For quantification this is not always appropriate. End groups are small and often shielded by larger resonances.
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2  What is the yield of the triblock copolymers after work up?
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3Why is the reaction performed at 90¡ãC?
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ÓÐûÓÐÊÔ¹ý different ratios of CuBr

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[ Last edited by lovehappy2008 on 2008-1-21 at 12:40 ]
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The authors rely heavily on 1HNMR characterization. For quantification this is not always appropriate. End groups are small and often shielded by larger resonances.
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PEO-TEMPO and PCL-TEMPO should therefore also be analyzed by MALDI MS In fig 6 and more particularly Fig 9, a clear shoulder and low molecular weight fraction are visible in the trace of the triblock copolymers. This raises doubts over the complete formation and purity of the triblock copolymer.  Most appropriate would be to analyze the samples with 2D chromatography. Another option would be to treat the samples with scavenger resin (azide and alkyne functional Merrifield resin for removal of unreacted alkynes and azides.)
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What is the yield of the triblock copolymers after work up?
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The triblock coupling efficiency as is calculated should be reformulated to show the ratio between the different blocks. This gives much more valuable information, because it can show the efficiency  of both coupling procedures. The calculation procedure can be shifted to the suppl. info.
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Why is the reaction performed at 90¡ãC? This one pot procedure could in principle also be performed at lower temperatures, which would yield another benefit toward other procedures. This experiment is strongly recommended. If it has already been investigated, then a comment on temperature effects should be included.
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For the one-pot procedure one equivalent of CuBr is used, which is in principle fully used by ATRNC. This could lead to problems with the click chemistry coupling. The authors should comment about this (is click chemistry much faster than ATRNC?, have they investigated different ratios of CuBr?).
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lovehappy2008

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[ Last edited by lovehappy2008 on 2008-1-22 at 00:15 ]
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