Organic Syntheses by Unknown
page 25 of 106 (23%)
page 25 of 106 (23%)
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Thorough washing of the crude aldehyde is particularly desirable, as it removes a reddish impurity which tends to distil over and color the product lemon yellow or sometimes even brownish yellow. When such a brownish product is obtained, it is quite necessary to make a second precipitation, as well as to observe the directions mentioned in the purification of the crude aldehyde, namely, to precipitate the first few grams and the last few grams of the aldehyde separately. The precaution of rejecting the first and last portions of the precipitate is unnecessary in the reprecipitation. In the reprecipitation of a deeply colored product, the portion of aldehyde at the end may be even purplish in color and particular care must be taken to keep this separate. Vigorous mechanical stirring must be employed during the precipitation of the crude aldehyde, as otherwise large lumps are formed which make washing difficult. A previous investigator has mentioned that the crude product must be dried before distilling. This, however, is unnecessary. If the aldehyde is dried before distilling, it is possible to use a 500-cc. distilling flask instead of a 1-l one. In purifying the aldehyde by dissolving in acid and reprecipitating, it is essential not to use stronger acid than that specified (1:6), as stronger acid causes a deepening of the color of the solution. If the concentrated acid, which is to be diluted and used in this procedure, does not have a sp. gr. of 1.19, it will be necessary to add the equivalent amount of weaker acid in order to dissolve the _p_-dimethylaminobenzaldehyde. In purifying the aldehyde, |
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