تفاعل #816389
ord-5f72f9533f9c4fe281afa03c6e1e88e8
معادلة التفاعل
glycine benzylester hydrochloride
K2CO3
chloroacetylchloride
→
material 1
N-(chloroacetyl)-glycine benzyl ester
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةThe mixture was warmed to room temperature
- 2أخرىThe two layers were separated
- 3استخلاصthe aqueous layer was extracted with CH2Cl2 (100 ml)
- 4غسيلwashed with H2O (100 ml), brine (100 ml)
- 5تجفيفdried (MgSO4)
- 6أخرىEvaporation of solvent
- 7أخرىafforded a light yellowish glassy solid
- 8أخرىThis was triturated with 250 ml of hexane
- 9أخرىThe colorless solid was collected
- 10أخرىdried
الإجراء التجريبي
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.