Reacción #1797514
ord-c0d4ee3aaa6a4e1da6d7c896e4cf81d1
Ecuación de reacción
Methyl 4-(3-(2-chloroethyl)ureido)benzoate
K2CO3
→
Methyl 4-(2-oxoimidazolidin-1-yl)benzoate
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1FiltraciónThe solid was filtered off
- 2Otrothe solvent was removed in vacuum
- 3workup.DISSOLUTIONThe crude product was dissolved in dichloromethane
- 4Otropurified on ISCO system (30% EtOAc in dichloromethane)
- 5Otroto give a pure product as a white crystalline (5.48 g, 75%)
Procedimiento
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).