반응 #347516

반응 방정식

4-phenoxyphenol

pyridine

4-nitrophenyl chloroformate

→

light yellow crystalline solid

수율 100.0%

Carbonic Acid (4-nitrophenyl)ester (4-phenoxy-phenyl)ester

수율 100.0%

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition the reaction
2. 2
   추출The reaction was extracted two times with 1N HCl, multiple times with saturated Na2CO3
3. 3
   건조dried (MgSO4)
4. 4
   기타the solvent removed under reduced pressure

실험 절차

A solution of 4-phenoxyphenol (50 g, 0.27 mol) and pyridine (22 mL, 0.27 mol) in 500 mL of methylene chloride was added under nitrogen dropwise over 1.5 hours to a solution of 4-nitrophenyl chloroformate (54 g, 0.27 mol) at room temperature. After the addition the reaction was stirred overnight at room temperature. The reaction was extracted two times with 1N HCl, multiple times with saturated Na2CO3, dried (MgSO4) and the solvent removed under reduced pressure to give 94.86 g of a light yellow crystalline solid. Recrystallization from methylene chloride-diisopropyl ether gave 69.13 g (73%) of the title compound as a light tan crystalline solid, mp 113°-115° C.

출처