反应详情

1.8 g of formanilide was dissolved in 50 ml of tetrahydrofuran, and 0.4 g of sodium hydride from which the oily matter had been removed before hand with n-hexane was slowly added to the resulting solution at 10° to 20° C. while cooling with ice water. To the suspension thus obtained was added 3.3 g of 4-chloro-2-methanesulfonyl-6-methoxypyrimidine, and the mixture was stirred for 1 hour at room temperature. Then, 15 ml of 4N hydrochloric acid was added, and reaction was effected for 1 hour under reflux. The reaction liquid was poured in water, extracted with ether, and the ether layer was washed with water, dried over magnesium sulfate, and then the ether was stripped by concentration. The residual crystals were recrystallized from n-hexane, and 4.0 g of 2-anilino-4-chloro-6-methoxypyrimidine was obtained (yield 87%). Melting point: 101°-103° C.

1. custom0.4 g of sodium hydride from which the oily matter had been removed before hand with n-hexane
2. additionwas slowly added to the resulting solution at 10° to 20° C.
3. temperaturewhile cooling with ice water
4. customTo the suspension thus obtained
5. customreaction
6. waitwas effected for 1 hour
7. temperatureunder reflux
8. customThe reaction liquid
9. extractionextracted with ether
10. washthe ether layer was washed with water
11. dry with materialdried over magnesium sulfate
12. concentrationthe ether was stripped by concentration
13. customThe residual crystals were recrystallized from n-hexane