반응 #1797514

반응 방정식

Methyl 4-(3-(2-chloroethyl)ureido)benzoate

K2CO3

→

Methyl 4-(2-oxoimidazolidin-1-yl)benzoate

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   여과The solid was filtered off
2. 2
   기타the solvent was removed in vacuum
3. 3
   workup.DISSOLUTIONThe crude product was dissolved in dichloromethane
4. 4
   기타purified on ISCO system (30% EtOAc in dichloromethane)
5. 5
   기타to give a pure product as a white crystalline (5.48 g, 75%)

실험 절차

Methyl 4-(3-(2-chloroethyl)ureido)benzoate (8.5 g, 33.1 mmol) was then stirred in N,N-dimethylformamide (80 ml) with K2CO3 (2.3 g, 16.7 mmol) at room temperature for 12 hours. The solid was filtered off and the solvent was removed in vacuum. The crude product was dissolved in dichloromethane and purified on ISCO system (30% EtOAc in dichloromethane) to give a pure product as a white crystalline (5.48 g, 75%): 1H NMR (400 MHz, CDCl3) δ 8.00 (d, 2H), 7.62 (d, 2H), 4.90 (br s, 1H), 3.97 (dd, 2H), 3.90 (s, 3H), 3.60 (dd, 2H). MS (ESI) m/z: Calculated: 220.08; Observed: 221.10 (M++1).

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