反应 #710485

反应方程式

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

收率 63.0%

溶剂

ethanol

ethyl acetate

反应条件

后处理

1. 1
   workup.ADDITIONwere added
2. 2
   其他liquid separation
3. 3
   洗涤the organic layer was washed with water
4. 4
   干燥dried over anhydrous magnesium sulfate
5. 5
   浓缩concentrated under reduced pressure
6. 6
   其他The organic layer was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)
7. 7
   其他to obtain the subject material
8. 8
   其他Amount obtained 625 mg (yield 63%)

实验过程

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%).

来源