反应详情

温度

10 °C

11.2 g (0.28 M) of 60% sodium hydride was suspended in 100 ml of N,N-dimethylformamide. While the suspension was cooled to 10° C. or lower in an ice water bath and stirred, there-to was dropwise added a solution of 29 g (0.14 M) of 3-methoxymethyl-2-nitrophenylacetonitrile dissolved in 100 ml of N,N-dimethylformamide. After the completion of the dropwise addition, the mixture was stirred at room temperature until there was no evolution of hydrogen. While the mixture was cooled to 10° C. or lower in an ice water bath and stirred, thereto was added 30 g (0.14 M) of 4,6-dimethoxy-2-methylsulfonylpyrimidine. The mixture was stirred at room temperature for 12 hours. The reaction mixture was poured into ice water. The mixture was acidified with 10% hydrochloric acid. The resulting crude crystals were collected by filtration, washed with water and a mixed solvent of ethanol and isopropyl ether to obtain 42 g (yield: 87%) of 2-(4,6-dimethoxypyrimidine-2-yl)-2-(3-methoxymethyl-2-nitrophenyl)acetonitrile as a reddish brown powder (melting point: 112 to 113° C.).

1. additionAfter the completion of the dropwise addition
2. stirringthe mixture was stirred at room temperature until there
3. temperatureWhile the mixture was cooled to 10° C. or lower in an ice water bath
4. stirringstirred
5. stirringThe mixture was stirred at room temperature for 12 hours
6. filtrationThe resulting crude crystals were collected by filtration
7. washwashed with water