反应 #1495574

反应方程式

diisopropyl diazodicarboxylate

3-(6-oxo-1,6-dihydropyridazin-3-yl)benzonitrile

[3-(5-methylpyrimidin-2-yl)phenyl]methanol

triphenylphosphine

→

3-{1-[3-(5-methylpyrimidin-2-yl)benzyl]-6-oxo-1,6-dihydropyridazin-3-yl}benzonitrile

溶剂

THF

反应条件

后处理

1. 1
   其他The reaction mixture is evaporated in vacuo, and 2-propanol
2. 2
   workup.ADDITIONis added to the residue
3. 3
   过滤The resultant precipitate is filtered off with suction
4. 4
   其他chromatographed on a silica gel column with dichloromethane/methanol as eluent

实验过程

8.3 147 μl (0.75 mmol) of diisopropyl diazodicarboxylate are added dropwise to a suspension of 98.6 mg (0.50 mmol) of 3-(6-oxo-1,6-dihydropyridazin-3-yl)benzonitrile, 100 mg (0.50 mmol) of [3-(5-methylpyrimidin-2-yl)phenyl]methanol and 197 mg (0.75 mmol) of triphenylphosphine in 3 ml of THF, and the resultant solution is stirred at room temperature for 18 hours. The reaction mixture is evaporated in vacuo, and 2-propanol is added to the residue. The resultant precipitate is filtered off with suction and chromatographed on a silica gel column with dichloromethane/methanol as eluent: 3-{1-[3-(5-methylpyrimidin-2-yl)benzyl]-6-oxo-1,6-dihydropyridazin-3-yl}benzonitrile (“A15”) as yellowish solid; ESI 380;

来源