Reacción #2304283

Ecuación de reacción

glycine benzylester hydrochloride

K2CO3

chloroacetylchloride

→

material 1

N-(chloroacetyl)-glycine benzyl ester

Disolventes

CH2Cl2

H2O

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe mixture was warmed to room temperature
2. 2
   OtroThe two layers were separated
3. 3
   Extracciónthe aqueous layer was extracted with CH2Cl2 (100 ml)
4. 4
   Lavadowashed with H2O (100 ml), brine (100 ml)
5. 5
   Secadodried (MgSO4)
6. 6
   OtroEvaporation of solvent
7. 7
   Otroafforded a light yellowish glassy solid
8. 8
   OtroThis was triturated with 250 ml of hexane
9. 9
   OtroThe colorless solid was collected
10. 10
    Otrodried

Procedimiento

To a suspension of glycine benzylester hydrochloride (25.2 g, 12.5 mmol, Aldrich) in CH2Cl2 (200 ml) was added a solution of K2CO3 (77 g, 55.8 mmol) in H2O (200 ml). The mixture was cooled to 0° C. and chloroacetylchloride (21.0 g, 18.6 mol, Aldrich) was added dropwise in 15 min. The mixture was warmed to room temperature and stirred for 2 h. The two layers were separated and the aqueous layer was extracted with CH2Cl2 (100 ml). The organic layers were combined and washed with H2O (100 ml), brine (100 ml), dried (MgSO4). Evaporation of solvent afforded a light yellowish glassy solid. This was triturated with 250 ml of hexane. The colorless solid was collected and dried to give 30.0 g of the material 1.

Fuente