Organic Syntheses by Unknown
page 9 of 106 (08%)
page 9 of 106 (08%)
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20'0). Commercial acetophenone contains variable quantities of impurities
which reduce the yield. By distilling commercial acetophenone with the help of a good still-head (preferably under diminished pressure) and using only the fraction which boils at 201-202'0 (76-77'0/10 mm.) greater quantities of benzalacetophenone can be obtained than by using the entire sample. Commercial benzaldehyde can be used in place of the purer product, but the amount used must be increased to make up for the impurities which are present. If the temperature is too low, or the stirring too slow, the product separates as an oil, which later solidifies in large lumps. If the temperature is allowed to rise above 30'0, secondary reactions diminish both the yield and the purity of the product. The most favorable temperature is 25'0. In recrystallizing benzalacetophenone, the alcohol should be saturated at 50'0. If the solution is saturated above this temperature, the benzalacetophenone tends to separate as an oil. The solution should be allowed to cool gradually, and should finally be chilled in a freezing mixture. 3. Other Methods of Preparation The methods for producing benzalacetophenone are: the action of acids on a mixture of benzaldehyde and acetophenone or on a solution of these substances in glacial acetic acid;[1] the condensation of benzaldehyde and acetophenone with a 30 per cent solution of sodium methylate at low temperatures;[2] the action of sodium hydroxide on an alcoholic solution of benzaldehyde and acetophenone.[3] |
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