反应 #1108427

反应方程式

Ethyl 2-fluoro-3-({[2-(morpholin-4-yl)pyrimidin-5-yl]oxy}methyl)benzoate

diisobutylaluminum hydride toluene

→

[2-fluoro-3-({[2-(morpholin-4-yl)pyrimidin-5-yl]oxy}methyl)phenyl]methanol

收率 85.1%

溶剂

toluene

反应条件

后处理

1. 1
   其他The reaction mixture was subjected to liquid separation by the addition of a 1 M aqueous NaOH solution and toluene
2. 2
   干燥The organic layer was dried over Na2SO4
3. 3
   浓缩concentrated under reduced pressure
4. 4
   其他The obtained residue was purified by silica gel column chromatography (hexane/EtOAc)

实验过程

Ethyl 2-fluoro-3-({[2-(morpholin-4-yl)pyrimidin-5-yl]oxy}methyl)benzoate (375 mg) was mixed with toluene (5 ml), followed by cooling to 0° C. A 1.01 M diisobutylaluminum hydride/toluene solution (3 ml) was added dropwise thereto, followed by stirring at the same temperature for 1 hour. The reaction mixture was subjected to liquid separation by the addition of a 1 M aqueous NaOH solution and toluene. The organic layer was dried over Na2SO4 and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/EtOAc) to obtain [2-fluoro-3-({[2-(morpholin-4-yl)pyrimidin-5-yl]oxy}methyl)phenyl]methanol (282 mg).

来源