反应详情

温度

40 °C

324 mg of (RS)-5-bromo-2-[4-(methylsulfinyl)phenylamino]pyrimidin-4-ol and 128 mg of sodium azide are suspended in 6 ml of methylene chloride and mixed drop by drop with 0.3 ml of concentrated sulfuric acid while being cooled with ice. The mixture is stirred for 36 hours at 40° C. The organic phase is decanted off, and the residue is stirred with ice water. The solid is suctioned off, washed twice with water and once with ethanol and dried. 266 mg (78.2% of theory) of the product with a melting point of 230° C. (decomposition) is obtained.

1. temperaturewhile being cooled with ice
2. customThe organic phase is decanted off
3. stirringthe residue is stirred with ice water
4. washwashed twice with water and once with ethanol
5. customdried
6. custom266 mg (78.2% of theory) of the product with a melting point of 230° C. (decomposition) is obtained