反应详情

温度

80 °C

In a 200 ml-three-necked flask, 1.77 g (12.3 mM) of heptanohydrazide, 3,23 g (13.0 mM) of 6-acetoxy-2-naphthoyl chloride prepared in the same manner as in Example 3 and 90 ml of dioxane were placed and heated to about 80° C. To the mixture, 5.0 ml of pyridine was added at about 80° C. under stirring, followed by heating to 90°-92° C. and stirring for 1 hour at 90°-92° C. After the reaction, the reaction mixture was cooled on an iced water bath and poured into 350 ml of iced water to precipitate a crystal. The crystal was recovered by filtration, followed by washing with water and recrystallization from a mixture solvent (acetoneethyl acetate) to obtain 3.23 g of N-heptanoyl-N'-(6-acetoxy-2-naphthoyl)hydrazine (Yield: 75.4 %) ##STR137##

1. temperatureby heating to 90°-92° C.
2. stirringstirring for 1 hour at 90°-92° C
3. customAfter the reaction
4. temperaturethe reaction mixture was cooled on an iced water bath
5. customto precipitate a crystal
6. filtrationThe crystal was recovered by filtration
7. washby washing with water and recrystallization from a mixture solvent (acetoneethyl acetate)