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note
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Elemental analysis of nitrogen (N) was conducted separately from carbon (C) and hydrogen (H). The analysis of N gave good agreement with the calculated one, although that of C was not within 0.4%. Thus, the sample was considered pure enough on the basis of the nitrogen analysis.
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note
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Chloroacetyl fluoride was prepared in 93% yield by reaction of chloroacetic acid (0.15 mol) with an equimolar amount of Fluolead reagent with no solvent in a fluoropolymer vessel at ice-bath temperature to room temperature for 2 h, followed by addition of powdered KF (0.2 mol) as a HF-trap. The volatile product was collected to a receiver cooled on a liquid nitrogen under vacuum (1∼4 mmHg) at a maximum temperature of 90 °C (oil bath). The liquid product (room temperature) was microfiltered through a small amount of KF to remove any last traces of HF that may have been present.
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