反应详情

温度

80 °C

20.6 g (0.1 mol) of N-dimethylaminomethyleneguanine obtained in Example 15, and 12.1 g (0.1 mol) of N,N-dimethylaniline were added to 38.3 g (0.25 mol) of phosphorus oxychloride, followed by stirring at 80° C. for 2 hours. After cooling, the reaction mixture was added to 500 ml of ice water, and then neutralized with 126.0 g (1.5 mol) of sodium hydrogen carbonate. The precipitating crystal was collected by filtration and then washed with 50 ml of water, subsequently with 50 ml of methanol to yield 18.0 g (0.08 mol) of a crystal of 2-dimethylaminomethyleneamino-6-chloropurine (yield 80%). Comparative Example (method disclosed in Japanese Patent Laid-Open No. 227583/1986)

1. temperatureAfter cooling
2. filtrationThe precipitating crystal was collected by filtration
3. washwashed with 50 ml of water, subsequently with 50 ml of methanol