反应详情

温度

80 °C

A solution of [2-(4-acetamido-phenyl-sulfanyl)-6-(4-methoxyphenyl)-pyrimidin-4-yl]-(5-methyl-2H-pyrazol-3-yl)-amine (100 mg, 2.24.10−4 mol) in dichloroethane (5 mL) is treated with 1M BBr3 in DCM (896 μL, 8.96.10−4 mol). The mixture is then heated at 80° C. for 4 hours before 1M BBr3 in DCM (896 μL, 8.96.10−4 mol) is added. The reaction mixture is then heated at 80° C. for a further 3 hours. The solvent is evaporated and methanol is added to the residue to quench any residual BBr3. The solvent is evaporated in vacuo and this evaporation step is repeated 3 times. 1M HCl(8 mL) is added to the solid residue and the suspension is stirred at room temperature for 15 hours. The solid is collected by filtration and suspended in a mixture of water/EtOH (3/1, 24 mL). The mixture is neutralized with NaHCO3 and stirred for 2 hours at room temperature. The solid is then collected by filtration, rinsed with water and with diethyl ether to give [2-(4-acetamido-phenyl-sulfanyl)-6-(4-hydroxyphenyl)-pyrimidin-4-yl]-(5-methyl-2H-pyrazol-3-yl)-amine.

1. additionis added
2. customThe solvent is evaporated
3. additionmethanol is added to the residue
4. customto quench any residual BBr3
5. customThe solvent is evaporated in vacuo
6. customthis evaporation step
7. addition1M HCl(8 mL) is added to the solid residue
8. filtrationThe solid is collected by filtration
9. additionsuspended in a mixture of water/EtOH (3/1, 24 mL)
10. stirringstirred for 2 hours at room temperature
11. filtrationThe solid is then collected by filtration
12. washrinsed with water and with diethyl ether