反応 #710485

反応方程式

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

収率 63.0%

溶媒

ethanol

ethyl acetate

反応条件

後処理

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

実験手順

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%).

出典