To
340 g. (6 moles) of dry, powdered potassium hydroxide (Note
1) in a
500-cc. short-necked round-bottomed flask (Note
2) is added
167 g. (1 mole) of β-chloropropionaldehyde acetal (p. 137). The mixture is shaken vigorously and attached at once to a
three-bulbed Glinsky or other suitable column, connected to a
water condenser set for distillation (Note
3). The flask is heated in an
oil bath at 210–220° until nothing more distils (Note
4). The distillate is transferred to a
separatory funnel and the lower aqueous layer is removed. The
acrolein acetal is dried over
10 g. of potassium carbonate, filtered, and distilled from a
modified Claisen flask (.htmFig. 2). The yield is
98 g. (
75 per cent of the theoretical amount) of a product which boils at
122–126°.
Fig. 2