反应详情

温度

130 °C

31.5 grams (0.1 mole) of 1,1'-ethylenebis(3,3,5,5-tetramethyl-2-piperazinone), prepared according to Example 6, E of U.S. Pat. No. 4,190,571 from N,N'-(2-amino-2-methylpropyl)ethylenediamine and acetone cyanohydrin, is dissolved in 102 grams (1.0 mole) of acetic anhydride. After three drops of concentrated sulfuric acid are added to the solution, the mixture is heated for four hours at 130° C. and then cooled to room temperature. Methylene chloride (200 ml.) is added to extract the product into an organic layer which is then washed successively with water and with saturated sodium bicarbonate solution and is finally dried over anhydrous magnesium sulfate. The solvent is removed in vacuo and the residual product is recrystallized from toluene to give 30.4 grams of the above-named product as a white solid, melting at 180°-183° C. (sintering at 170° C.).

1. temperaturecooled to room temperature
2. extractionto extract the product into an organic layer which
3. washis then washed successively with water and with saturated sodium bicarbonate solution
4. dry with materialis finally dried over anhydrous magnesium sulfate
5. customThe solvent is removed in vacuo
6. customthe residual product is recrystallized from toluene