تفاعل #710484

معادلة التفاعل

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

المردود 56.0%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىwas returned to room temperature
2. 2
   ترشيحsubjected to suction filtration
3. 3
   أخرىto remove insoluble materials
4. 4
   workup.ADDITIONEthyl acetate and water were added
5. 5
   أخرىliquid separation
6. 6
   تجفيفthe organic layer was dried over anhydrous magnesium sulfate
7. 7
   تركيزconcentrated under reduced pressure
8. 8
   أخرىpurified with silica gel column chromatography (hexane:ethyl acetate=1:1)
9. 9
   أخرىto obtain the subject material
10. 10
    أخرىAmount obtained 81 mg (yield 56%)

الإجراء التجريبي

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%).

المصدر