반응 #81774

반응 방정식

2,4,6-triiodophenol

diethyl bromomalonate

potassium carbonate

→

product

수율 64.0%

Diethyl 2-(2,4,6-Triiodophenoxy)-1,3-propanedioate

수율 64.0%

용매

dimethylformamide

반응 조건

후처리

1. 1
   온도The mixture was cooled
2. 2
   농축concentrated in vacuo
3. 3
   추출the oily product was extracted with ethyl acetate (1×300 ml), 3×100 ml)
4. 4
   건조The combined ethyl acetate extracts were dried (MgSO4)
5. 5
   농축concentrated in vacuo to a dark oil
6. 6
   기타The oil was purified by chromatography (eluted by hexanes to 20% diethyl ether in hexanes)

실험 절차

A stirred mixture of 70.8 g (0.15 mol) of 2,4,6-triiodophenol, 39.0 g (0.15 mol) of diethyl bromomalonate and 20.7 g (0.15 mol) of milled anhydrous potassium carbonate in 200 ml of dry dimethylformamide was heated at 100° C. under argon for 5 hours. The mixture was cooled and concentrated in vacuo. The resulting residue was combined with 300 ml of ice-cold water and the oily product was extracted with ethyl acetate (1×300 ml), 3×100 ml). The combined ethyl acetate extracts were dried (MgSO4) and concentrated in vacuo to a dark oil. The oil was purified by chromatography (eluted by hexanes to 20% diethyl ether in hexanes) to yield 60.2 g (64%) of product as a light cream-colored solid.

출처