反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
484 mg of potassium carbonate and 456 mg of methyl iodide were added to a 5-mL N,N-dimethylformamide solution containing 1.00 g of the 7-chloro-3-(2,6-dichlorophenyl)-4-imino-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one obtained in Production Example 1, and the mixture was stirred for 1 hour at room temperature. The reaction mixture was added to ethyl acetate and a 0.5 N hydrochloric acid aqueous solution with stirring to separate the organic layer. After washing with saturated saline, the solution was dried with anhydrous sodium sulfate, and the solvent was distilled away. The crude product was solidified using chloroform-methanol-hexane, and 700 mg of a yellow solid was obtained as a subject compound.
WORKUP
后处理
- customobtained in Production Example 1
- customto separate the organic layer
- washAfter washing with saturated saline
- dry with materialthe solution was dried with anhydrous sodium sulfate
- distillationthe solvent was distilled away