反应 #1755518

反应方程式

3-aminobenzaldehyde

2-fluoro-5-trifluoromethylphenyl isocyanate

potassium hydrogen sulfate

→

aldehyde

收率 57.0%

1-(2-fluoro-5-trifluoromethylphenyl)-3-(3-formylphenyl)urea

收率 57.0%

溶剂

DCE

反应条件

后处理

1. 1
   workup.ADDITIONis treated in a CEM Discover microwave oven at 100° C. for 10 minutes (power 90)
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

A mixture of 484 mg of 3-aminobenzaldehyde (4 mmol) (polymerized form) and 290 μl of 2-fluoro-5-trifluoromethylphenyl isocyanate in 4 ml of DCE is treated in a CEM Discover microwave oven at 100° C. for 10 minutes (power 90). 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. 740 mg of the expected aldehyde (yield=57%) are obtained in an LC/MS purity of 82%. The crude product is used directly for the following steps. ([M+H]+): 327. RT=4.28 min (acetonitrile/water gradient from 30% to 90%—Method B).

来源