반응 #1755519

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3-aminobenzaldehyde

2-fluorophenyl isocyanate

potassium hydrogen sulfate

→

aldehyde

수율 83.7%

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

수율 83.7%

용매

DCE

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후처리

1. 1
   기타The product was prepared
2. 2
   온도After cooling
3. 3
   추출extracted with twice 50 ml of ethyl acetate
4. 4
   세척The combined organic phases are washed with water
5. 5
   건조dried over sodium sulfate
6. 6
   기타evaporated

실험 절차

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).

출처