反应 #566683

反应方程式

solution

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

3-aminopyridine

triethylamine

→

desired product

收率 52.3%

4-chloro-N-(2,2,2-trichloro-1-(((3-pyridinylamino)carbothioyl)amino)ethyl)benzamide

收率 52.3%

溶剂

THF

ethyl acetate

反应条件

后处理

1. 1
   洗涤washed with water (2×10 mL) and brine (10 mL)
2. 2
   干燥The organic portion was dried (MgSO4)
3. 3
   过滤filtered
4. 4
   浓缩concentrated
5. 5
   其他to provide an oily residue which
6. 6
   其他was purified by flash chromatography (elution with 5% ethanol/hexanes)

实验过程

A solution of Example 45A (239mg, 0.695 mmol) and 3-aminopyridine (65 mg, 0.69 mmol) in THF (4 mL) at ambient temperature was treated with triethylamine (1.66 mL, 1.18 mmol). The mixture was stirred for 3 hours, diluted with ethyl acetate (20 mL), and washed with water (2×10 mL) and brine (10 mL). The organic portion was dried (MgSO4), filtered, and concentrated to provide an oily residue which was purified by flash chromatography (elution with 5% ethanol/hexanes) to provide 158 mg of the desired product as an off-white solid.

来源