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Organic Lab Reactions 206

Organic Lab Reactions 206 - REDUCTION OF BENZALDEHYDE 201...

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REDUCTION OF BENZALDEHYDE 201 of aluminum and 500 cc. of isopropyl alcohol, are added 210 g. (3 moles) of crotonaldehyde and 1 1. of dry isopropyl alcohol. A 2-1. round-bot- tomed flask is used, equipped with an 80-cm. Vigreux column, the upper end of which is connected to a water condenser set for downward dis- tillation. The~mixture is heated with an oil bath, and the acetone slowly distils as it is formed. The temperature of the distillate is maintained at 60 to 70° (bath 110°), and when the distillate no longer gives a test for acetone (eight to nine hours) most of the remaining isopropyl alcohol is distilled under reduced pressure.* The residue is cooled to 40° and slowly hydrolyzed (cooling as neces- sary) with 900 cc. of cold 6 JV sulfuric acid, prepared from 145 cc. of concentrated sulfuric acid and 790 cc. of water. The oily layer is sep- arated, washed once with water, and distilled at 60-70° while the pres- Bure is lowered slowly from about 275 mm. to 65 mm. Finally the dis- tillation is continued to 100° and 20 mm.
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