반응 #440181

반응 방정식

HCl

4,4′-dihydroxybiphenyl

acrylic acid 6-iodohexyl ester

potassium carbonate

→

Acrylic acid 6-(4′-hydroxybiphenyl-4-oxy)hexyl ester

용매

DMF

반응 조건

후처리

1. 1
   추출extracted with ether (3×200 ml)
2. 2
   세척The combined organic extracts were washed with saturated NaCl solution (200 ml)
3. 3
   건조dried over magnesium sulfate
4. 4
   여과filtered
5. 5
   기타evaporated to dryness
6. 6
   기타The crystalline residue obtained
7. 7
   기타was purified on silica-gel column (CH2Cl2, CH2Cl2/Et2O:19/1)

실험 절차

A solution of 4,4′-dihydroxybiphenyl (3.72 g, 20 mmol), acrylic acid 6-iodohexyl ester (4.21 g, 15 mmol) and potassium carbonate (2.07 g, 15 mmol) in DMF (50 ml) was stirred overnight at room temperature and under argon atmosphere. The reaction mixture was then poured into HCl 3N (100 ml) and extracted with ether (3×200 ml). The combined organic extracts were washed with saturated NaCl solution (200 ml), dried over magnesium sulfate, filtered and evaporated to dryness. The crystalline residue obtained was purified on silica-gel column (CH2Cl2, CH2Cl2/Et2O:19/1). This gave acrylic acid 6-(4′-hydroxybiphen-4-yloxy-)hexyl ester as white crystalline material. Yield 2.5 g.

출처