huaxue（huaxue）.docVIP

huaxue（huaxue） I. experimental purpose 1. Master the principle and method of preparing acetaniline from aniline acetylation. 2. Master the principle of fractionation and the installation and operation of fractionation devices. 3. Consolidate the operation method of recrystallization. 2. Experimental principle Reactive: The role of aromatic acylation in organic synthesis: (1) acetylation is often used to protect beramine and secondary amine functional groups to reduce the sensitivity of aromatic amine to oxidative reagents. (2) after acylation of amino, reduces the amino electrophilic substitution (especially the halide) in the activated ability, make it by the first class I strong positioning base into a medium strength of the ith class localization, make it become a useful reaction replaced by multiple replaced one yuan. (3) because of the spatial effect of acetyl groups, it is often selective to generate the opposite product. (4) in some cases, acylation can avoid unnecessary reactions between amino and other functional groups or reagents such as RCOCl, -so2cl, HNO2, and so on. The acyl group of amino groups can be removed under the catalysis of acids or bases. Aryl chloride, acid anhydride or glacial acetic acid is used to make acylation, and the use of glacial acetic acid is easy and cheap, but it requires a long reaction time, which is suitable for larger preparation. Although acetic anhydride is generally a better acylated reagent than acyl chloride, when it is acylated with free amine and pure acetic anhydride, it is often accompanied by the formation of a by-product of diacetamide [ArN (COCH3) 2]. 3. Operation steps Experimental procedures and procedures 1. Feeding: In 25 mL round bottom flask, add 10 mL of aniline, 1.5 mL glacial acetic acid and zinc powder (0.01 g) and then put on a short stinging fractionating column, the top with a thermometer, branch by branch lead tube connected to accept bottle, bottle accept external use cold water to cool. 2. The r