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4 to an aqueous solution may be a basic principle, however, only solids were handled and the reaction vessel was closed not until bubbling had stopped.
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We found a strong influence of the reactivity and type of Pd catalyst to the level of deuterium incorporation and therefore all reactions were performed with Pd/C (10% Pd) K-02105 purchased from Heraeus.
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2O (99% D). The mixture was stirred for approximately 30 s and the tube was sealed (remark: the reaction vessel was closed not until bubbling had stopped) and heated to 130 °C for 18 h. The mixture was cooled to r.t. and 3 mL MeCN were added. The catalyst was separated by filtration. The product was purified by chromatography if necessary and analyzed by NMR and LC-MS.
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33747041571
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max was determined by an Agilent 1100 System LC-MS instrument.
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62
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