反应详情

A solution of 2-(2-cyanoethyl) 3,3-diaminopropenoic acid ethyl ester described in Preparation Example A-12 (0.55 g, 3 mmol) in tetrahydrofuran (7 mL) was added dropwise to a suspension of sodium hydride (208 mg, 5.2 mmol, 60% in oil) in tetrahydrofuran (7 mL), and the solution was stirred for 19 hours 20 minutes under reflux. After the reaction was completed, the reaction solution was poured into an ice water, which was then extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, then, concentrated to obtain the title compound as a crude product (0.188 g, 1 mmol, 34%).

1. temperatureunder reflux
2. extractionwas then extracted with ethyl acetate
3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
4. concentrationconcentrated