反应 #1755519

反应方程式

3-aminobenzaldehyde

2-fluorophenyl isocyanate

potassium hydrogen sulfate

→

aldehyde

收率 83.7%

1-(2-fluorophenyl)-3-(3-formylphenyl)urea

收率 83.7%

溶剂

DCE

反应条件

后处理

1. 1
   其他The product was prepared
2. 2
   温度After cooling
3. 3
   萃取extracted with twice 50 ml of ethyl acetate
4. 4
   洗涤The combined organic phases are washed with water
5. 5
   干燥dried over sodium sulfate
6. 6
   其他evaporated

实验过程

The product was prepared as described in Example 2, starting with 484 mg of 3-aminobenzaldehyde (4 mmol) (polymerized form) and 548 mg of 2-fluorophenyl isocyanate in 4 ml of DCE. After cooling, the mixture is poured into 100 ml of saturated potassium hydrogen sulfate solution and extracted with twice 50 ml of ethyl acetate. The combined organic phases are washed with water, dried over sodium sulfate and evaporated. 864 mg of the expected aldehyde are isolated in the form of a gum, in an LC/MS purity of 77%. A crystallized fraction is obtained after trituration from ethyl ether. 165 mg of solid are isolated ([M+H]+): 259. RT=4.28 min (acetonitrile/water gradient from 5% to 85%—Method B).

来源