Organic Syntheses by Unknown
page 30 of 106 (28%)
page 30 of 106 (28%)
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one above and one below the tube leading to the potassium carbonate tube.
The long return tube to the flask may be constructed with a rubber joint very near the carbonate tube and one near the flask. 3. Other Methods of Preparation Ethyl oxalate has been prepared in poor yields by the following methods: by distilling a mixture of anhydrous oxalic acid and absolute alcohol;[1] by heating a mixture of anhydrous oxalic acid and 97 per cent alcohol under a reflux condenser and fractionating the resulting mixture;[2] by distilling a mixture of anhydrous oxalic acid and absolute alcohol, the vapor of absolute alcohol being passed simultaneously into the mixture;[3] by allowing a saturated solution of oxalic acid in alcohol to stand for a long time at 40-50'0.[4] A good yield has been obtained by Anschutz[5] by a method involving saturation of a mixture of crystallized oxalic acid and alcohol with hydrogen chloride, removal of the alcohol and water by distillation under reduced pressure, and repetition of the treatment with the alcohol and hydrogen chloride, the process being carried out several times. [1] Jahresb. 1861, 598. [2] J prakt. Chem. (2), 34, 500 (1886). [3] Monatsh. 17, 614 (1896). |
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