反应 #816389

反应方程式

glycine benzylester hydrochloride

K2CO3

chloroacetylchloride

→

material 1

N-(chloroacetyl)-glycine benzyl ester

溶剂

CH2Cl2

H2O

反应条件

后处理

1. 1
   温度The mixture was warmed to room temperature
2. 2
   其他The two layers were separated
3. 3
   萃取the aqueous layer was extracted with CH2Cl2 (100 ml)
4. 4
   洗涤washed with H2O (100 ml), brine (100 ml)
5. 5
   干燥dried (MgSO4)
6. 6
   其他Evaporation of solvent
7. 7
   其他afforded a light yellowish glassy solid
8. 8
   其他This was triturated with 250 ml of hexane
9. 9
   其他The colorless solid was collected
10. 10
    其他dried

实验过程

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.

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