Reaktion #816389

Reaktionsgleichung

glycine benzylester hydrochloride

K2CO3

chloroacetylchloride

→

material 1

N-(chloroacetyl)-glycine benzyl ester

Lösungsmittel

CH2Cl2

H2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was warmed to room temperature
2. 2
   SonstigeThe two layers were separated
3. 3
   Extraktionthe aqueous layer was extracted with CH2Cl2 (100 ml)
4. 4
   Waschenwashed with H2O (100 ml), brine (100 ml)
5. 5
   Trocknendried (MgSO4)
6. 6
   SonstigeEvaporation of solvent
7. 7
   Sonstigeafforded a light yellowish glassy solid
8. 8
   SonstigeThis was triturated with 250 ml of hexane
9. 9
   SonstigeThe colorless solid was collected
10. 10
    Sonstigedried

Vorschrift

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.

Quelle