反应 #710484

反应方程式

N-[1-((6-chloropyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-2,2,2-trifluoroethanethioamide

methylamine

→

N-[1-((6-chloropyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-2,2,2-trifluoro-N′-methylacetimidamide

收率 56.0%

溶剂

methanol

反应条件

后处理

1. 1
   其他was returned to room temperature
2. 2
   过滤subjected to suction filtration
3. 3
   其他to remove insoluble materials
4. 4
   workup.ADDITIONEthyl acetate and water were added
5. 5
   其他liquid separation
6. 6
   干燥the organic layer was dried over anhydrous magnesium sulfate
7. 7
   浓缩concentrated under reduced pressure
8. 8
   其他purified with silica gel column chromatography (hexane:ethyl acetate=1:1)
9. 9
   其他to obtain the subject material
10. 10
    其他Amount obtained 81 mg (yield 56%)

实验过程

150 mg (0.45 mmol) of the N-[1-((6-chloropyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-2,2,2-trifluoroethanethioamide (1-20) synthesized by the method in Synthetic Example 4 was dissolved in 5 ml of methanol, 105 μl (42 mg, 1.36 mmol) of methylamine (40% methanol solution) and 124 mg (0.45 mmol) of silver carbonate were added thereto, and the resulting mixture was stirred at 50° C. for 1 hour. After the reaction was completed, the reaction solution was returned to room temperature and subjected to suction filtration by using celite to remove insoluble materials. Ethyl acetate and water were added thereto to perform liquid separation, and the organic layer was dried over anhydrous magnesium sulfate, then concentrated under reduced pressure and purified with silica gel column chromatography (hexane:ethyl acetate=1:1) to obtain the subject material. Amount obtained 81 mg (yield 56%).

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