反应 #566682

反应方程式

diethyl ether

solution

4-chloro-N-(1,2,2,2-tetrachloroethyl)benzamide

potassium thiocyanate

→

desired product

收率 0.1%

4-chloro-N-(2,2,2-trichloro-1-isothiocyanatoethyl)benzamide

收率 0.1%

溶剂

acetone

反应条件

后处理

1. 1
   其他solids were removed by filtration
2. 2
   浓缩The filtrate was concentrated
3. 3
   其他to provide a yellow residue
4. 4
   其他the suspension was sonicated
5. 5
   过滤filtered
6. 6
   其他Concentration of the residue and purification
7. 7
   其他by recrystallization (25% ethyl acetate/hexanes)

实验过程

A solution of Example 41B (1.91 g, 6.31 mmol) in acetone (30 mL) at ambient temperature was treated with potassium thiocyanate (1.38 g, 14.1 mmol). The mixture was stirred for 6 hours and solids were removed by filtration. The filtrate was concentrated to provide a yellow residue. The residue was treated with diethyl ether, and the suspension was sonicated and filtered. Concentration of the residue and purification by recrystallization (25% ethyl acetate/hexanes) provided 1.85 mg of the desired product as a yellow solid.

来源