反应 #2549

反应方程式

THF

n-butyl lithium

morpholine

4-chloromethyl-N-(2-methoxyphenyl)benzamide

→

title compound

收率 39.2%

N-(2-Methoxyphenyl)-4-morpholinomethylbenzamide

收率 39.2%

溶剂

water

ether

反应条件

后处理

1. 1
   温度with cooling in an ice bath
2. 2
   workup.STIRRINGstirring for 2.5 hours at 60° C.
3. 3
   萃取extracted with ethyl acetate
4. 4
   其他After removing insoluble materials
5. 5
   过滤by filtration
6. 6
   洗涤the organic layer was washed with water and saturated brine
7. 7
   干燥dried on anhydrous sodium carbonate
8. 8
   其他Thereafter, the solvent was removed by evaporation
9. 9
   其他the resulting residue was purified

实验过程

In an atmosphere of argon, morpholine (192 mg, 2.2 mmol) was dissolved in ether (5 ml) to which, with cooling in an ice bath, was subsequently added n-butyl lithium (1.45 ml, 1.52M, 2.2 mmol). After 5 minutes of stirring at room temperature, to this was added 4-chloromethyl-N-(2-methoxyphenyl)benzamide (276 mg, 1.0 mmol) at the same temperature. After adding THF (5 ml) and stirring for 2.5 hours at 60° C., the reaction solution was mixed with water (20 ml) and extracted with ethyl acetate. After removing insoluble materials by filtration, the organic layer was washed with water and saturated brine and then dried on anhydrous sodium carbonate. Thereafter, the solvent was removed by evaporation, and the resulting residue was purified by subjecting it to a silica gel column chromatography (ether) to obtain 128 mg (39.2%) of the title compound in the form of light yellow solid.

来源