반응 #2304283

반응 방정식

glycine benzylester hydrochloride

K2CO3

chloroacetylchloride

→

material 1

N-(chloroacetyl)-glycine benzyl ester

용매

CH2Cl2

H2O

반응 조건

후처리

1. 1
   온도The mixture was warmed to room temperature
2. 2
   기타The two layers were separated
3. 3
   추출the aqueous layer was extracted with CH2Cl2 (100 ml)
4. 4
   세척washed with H2O (100 ml), brine (100 ml)
5. 5
   건조dried (MgSO4)
6. 6
   기타Evaporation of solvent
7. 7
   기타afforded a light yellowish glassy solid
8. 8
   기타This was triturated with 250 ml of hexane
9. 9
   기타The colorless solid was collected
10. 10
    기타dried

실험 절차

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.

출처