反应 #1951077

反应方程式

2,6-Dichlorophenyl isothiocyanate

2-(4-amino-2-cyano-3-methylamino-phenyl)-2-methyl-3-oxo-butyric acid ethyl ester

→

2-[4-cyano-2-(2,6-dichloro-phenylamino)-3-methyl-3H-benzoimidazol-5-yl]-2-methyl-3-oxo-butyric acid ethyl ester

收率 54.0%

溶剂

THF

反应条件

后处理

1. 1
   其他equipped with a magnetic stir bar
2. 2
   workup.STIRRINGthe reaction stirred for an additional 14 h
3. 3
   过滤The resultant brown slurry was filtered through celite
4. 4
   洗涤washed with THF
5. 5
   浓缩The filtrate was concentrated
6. 6
   其他the residue triturated with diethyl ether

实验过程

2,6-Dichlorophenyl isothiocyanate (3.46 g, 17.0 mmol), THF (100 mL), and 2-(4-amino-2-cyano-3-methylamino-phenyl)-2-methyl-3-oxo-butyric acid ethyl ester (4.91 g, 17.0 mmol), were added to a 250 mL round bottom flask equipped with a magnetic stir bar and the reaction was stirred at room temperature. After 2 hours, mercuric oxide (4.04 g, 18.7 mmol) was added and the reaction stirred for an additional 14 h. The resultant brown slurry was filtered through celite and washed with THF. The filtrate was concentrated and the residue triturated with diethyl ether to provide 2-[4-cyano-2-(2,6-dichloro-phenylamino)-3-methyl-3H-benzoimidazol-5-yl]-2-methyl-3-oxo-butyric acid ethyl ester (4.2 g, 54%) as a gray solid, which was used without further purification.

来源