反应 #587368

反应方程式

N,N-Dimethylcarbamoyl chloride

1-(4-bromo-2-fluorophenyl)methanamine

triethylamine

→

N′-(4-bromo-2-fluorobenzyl)-N,N-dimethylurea

溶剂

methylene chloride

反应条件

后处理

1. 1
   其他the ice-water bath was removed
2. 2
   洗涤The mixture was washed with water and brine
3. 3
   干燥The organic layer was dried over Na2SO4
4. 4
   过滤filtered
5. 5
   浓缩concentrated under reduced pressure
6. 6
   其他The residue (253 mg, 91.9%) was directly used in next step without further purification

实验过程

N,N-Dimethylcarbamoyl chloride (101 μL, 1.1 mmol) was added to a solution of 1-(4-bromo-2-fluorophenyl)methanamine (0.204 g, 1.0 mmol) and triethylamine (148.1 μL, 1.10 mmol) in methylene chloride (5 mL) at 0° C., followed by 4-dimethylaminopyridine (0.012 g, 0.1 mmol). After 10 min, the ice-water bath was removed and the mixture was stirred overnight at RT. The mixture was washed with water and brine. The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue (253 mg, 91.9%) was directly used in next step without further purification. LCMS: (M+H)=276.9/274.9.

来源