反应 #1797514

反应方程式

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

K2CO3

→

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

溶剂

N,N-dimethylformamide

反应条件

后处理

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

实验过程

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).

来源