반응 #57525

반응 방정식

3-iodophenol

magnesium chloride

triethylamine

paraformaldehyde

ammonium chloride

→

solid

수율 160.1%

4-Iodo-2-hydroxy-benzaldehyde

수율 160.1%

용매

acetonitrile

반응 조건

후처리

1. 1
   온도The reaction mixture was refluxed overnight
2. 2
   기타The resultant red precipitate was removed by filtration
3. 3
   추출the filtrate was extracted with ethyl acetate
4. 4
   workup.DISSOLUTIONThe precipitate was dissolved in methanol
5. 5
   workup.ADDITIONadded to the combined organic extracts, which
6. 6
   건조were then dried over magnesium sulfate
7. 7
   기타The solvent was removed under reduced pressure

실험 절차

To a solution of 3-iodophenol (3.00 g, 13.6 mmol) in acetonitrile (50 mL) was added magnesium chloride (3.89 g, 40.9 mmol), triethylamine (7.6 mL, 55 mmol), and paraformaldehyde (1.64 g, 55 mmol). The reaction mixture was refluxed overnight, then neutralized with saturated aqueous ammonium chloride. The resultant red precipitate was removed by filtration, and the filtrate was extracted with ethyl acetate. The precipitate was dissolved in methanol and added to the combined organic extracts, which were then dried over magnesium sulfate. The solvent was removed under reduced pressure to provide an orange solid (5.4 g) as the crude product. This material was used in the subsequent step without further purification.

출처