- Purification of Acetic anhydride
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Adequate purification of (CAS NO.) can usually be obtained by fractional distn through an efficient column. can be removed by prior refluxing with CaC2 or with coarse Mg filings at 80-90 °C for Sdays, or by distn from a large excess of quinoline (1 % AcOH in quinoline) at 75mm pressure. Acetic anhydride can also be dried by standing with Na wire for up to a week, removing the Na and distilling from it under vacuum. (Na reacts vigorously with acetic anhydride at 65-70°C). Dippy and Evans let the anhydride (500g) stand over P2O5 (50g) for 3h, then decanted it and stood it with ignited K2CO3 for a further 3h. The supernatant liquid was distd and the fraction b 136-138°C, was further dried with P2O5 for 12h, followed by shaking with ignited K2CO3, before two further distns through a five-section Young and Thomas fractionating column. The final material distd at 137.8-138.0°C. Can also be purified by azeotropic distn with toluene: the azeotrope boils at 100.6°C. After removal of the remaining toluene, the anhydride is distd [sample had a specific conductivity of 5×10-9 ohm-1cm-1].
RapM procedure: Shake with P2O5, separate, shake with dry K2CO3 and fractionally distil.
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