Реакция #710485

Уравнение реакции

hydroxylamine hydrochloride

triethylamine

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

hydrochloric acid

→

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

Выход 63.0%

Растворители

ethanol

ethyl acetate

Условия реакции

Обработка

1. 1
   workup.ADDITIONwere added
2. 2
   Другоеliquid separation
3. 3
   Промывкаthe organic layer was washed with water
4. 4
   Сушкаdried over anhydrous magnesium sulfate
5. 5
   Концентрированиеconcentrated under reduced pressure
6. 6
   ДругоеThe organic layer was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)
7. 7
   Другоеto obtain the subject material
8. 8
   ДругоеAmount obtained 625 mg (yield 63%)

Методика

25 ml of ethanol was added to 1.00 g (3.00 mmol) of the N-[1-((6-chloropyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-2,2,2-trifluoroethanethioamide (1-20) 1 synthesized by the method in Synthetic Example 4, 1.04 g (15.0 mmol) of hydroxylamine hydrochloride and 2.00 ml (1.50 g, 15.0 mmol) of triethylamine were added thereto in sequence, and the resulting mixture was stirred at 50° C. for 21.5 hours. After the reaction was completed, ethyl acetate and 1% hydrochloric acid were added to the reaction solution to perform liquid separation, and the organic layer was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The organic layer was purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to obtain the subject material. Amount obtained 625 mg (yield 63%).

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