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4. The pD of the reaction mixture was measured before the initiation of the reaction and after the reaction was complete. The pD was obtained by adding 0.4 to the observed pH reading (see ref 8b).
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23
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0041995655
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note
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3 at 7.27 ppm. The NMR spectrum of the α-methylene protons was complicated by coupling to the methylene protons at the C3 position. To simplify the spectrum of the α-methylene protons, the protons in the C3 position (at 2 ppm) were subjected to inverse gated homonuclear decoupling (see refs 7e and 9b).
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0041494658
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CHD). The area of the triplet was calculated by multiplying the area of the measurable peak by three.
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-
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28
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0042997279
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note
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(a) We have treated the four a-protons of 1 as being all equivalent. This analysis disregards the two potential dideuterated products that can be formed; however, these experiments are followed for exchange of 20% of the total α-protons, which is approximately 40% of the first α-proton of a single methylene unit. Similar experiments with acetone (see ref 7a) did not observe complicating dideuteration with similar incorporation percentages, and we did not observe any evidence suggesting this complication was occurring.
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0001327410
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0041995654
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2O
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2O.
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