反应详情

温度

77.5 °C

A mixture of 6-chloro-2-(chloromethyl)imidazo[1,2-α]pyridine (Example 4, step 1, 0.857 g), 3-fluoro-4-(piperazin-1-yl)benzonitrile (1.039 g), triethylamine (0.75 mL), and THF (6 mL) is stirred for 3 h at 75-80° C. The mixture is then concentrated under reduced pressure and the residue is partitioned between dichloromethane and saturated sodium bicarbonate. The combined organic layers are dried with MgSO4 and concentrated under reduced pressure. The residue is chromatographed on silica gel using methanol/dichloromethane (4/96). The appropriate fractions are combined and concentrated. Ethyl ether is added to the residue and the resulting solid is collected, washed with additional ethyl ether, and dried under reduced pressure to give 1.25 g of the title compound. A portion of this material is recrystallized from ethyl acetate; mp 132-133° C. ; IR (mineral oil) 1255, 1513, 1246, 801, 1504 cm-1 ; 1H NMR (CDCl3) δ2.74, 3.26, 3.77, 6.90, 7.13, 7.25, 7.34, 7.53, 8.13.

1. concentrationThe mixture is then concentrated under reduced pressure
2. customthe residue is partitioned between dichloromethane and saturated sodium bicarbonate
3. dry with materialThe combined organic layers are dried with MgSO4
4. concentrationconcentrated under reduced pressure
5. customThe residue is chromatographed on silica gel
6. concentrationconcentrated
7. additionEthyl ether is added to the residue
8. customthe resulting solid is collected
9. washwashed with additional ethyl ether
10. customdried under reduced pressure