反応 #1797514

反応方程式

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

K2CO3

→

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

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   ろ過The solid was filtered off
2. 2
   その他the solvent was removed in vacuum
3. 3
   workup.DISSOLUTIONThe crude product was dissolved in dichloromethane
4. 4
   その他purified on ISCO system (30% EtOAc in dichloromethane)
5. 5
   その他to give a pure product as a white crystalline (5.48 g, 75%)

実験手順

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).

出典