Organic Syntheses, CV 3, 371
Submitted by C. G. Alberti and R. Sollazzo.
Checked by Miriam Sharp, V. L. Stromberg, and E. C. Horning.
1. Procedure
In a
1-l. three-necked round-bottomed flask fitted with a
reflux condenser, a
mechanical stirrer, and a
thermometer dipping below the surface of the mixture are placed
158 g. (2.8 moles) of acrolein (Note
1),
500 ml. of absolute ethanol, and
10 g. of ammonium chloride (Note
2). The material is stirred for 1 hour without external heating; the temperature of the mixture should rise to about 30°. Over a 3-hour period the temperature is raised to 80°, and the mixture is maintained at this temperature for an additional hour. The flask is then cooled, and anhydrous
sodium or magnesium sulfate is added as a drying agent.
After 24 hours the mixture is filtered and distilled under reduced pressure through a good column (Note
3). The following fractions are collected (Note
4):
2. Notes
3. A
1-m. Fenske column packed with 3/32-in. glass helices was employed by the submitters.
4.
Ammonium chloride separates during the distillation. It is advisable to decant the liquid into a clean flask for distillation of the last two fractions.
3. Discussion
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