反应详情

To a suspension of 50% sodium hydride (7.4 g) in anhydrous dioxane (50 ml), under nitrogen, a solution of diethyl oxalate (34.5 g) in anhydrous dioxane (20 ml) and then a solution of 2a,3,4,5-tetrahydro-acenaphthen-1-one (20.4 g) in anhydrous dioxane (130 ml) are added under stirring at room temperature. The reaction mixture is kept under stirring at a temperature varying between about 25° C. and about 45° C. for 4 hours, then it is diluted with ice water (1500 ml) and acidified to pH 4 with 2N HCl. The precipitate is filtered, washed with water and then purified by treatment with methanol to give 2-ethoxalyl-2a,3,4,5-tetrahydro-acenaphthen-1-one (30.8 g), m.p. 92°-94° C., wich is reacted with methylhydrazine (5.7 g) in acetic acid (300 ml) at 50° C. for 1 hour.

1. stirringunder stirring at a temperature
2. filtrationThe precipitate is filtered
3. washwashed with water
4. custompurified by treatment with methanol