반응 #50757

반응 방정식

2-(5-amino-1,2,4-thiadiazol-3-yl)-2-fluoromethoxyiminoacetic acid hydrate

phosphorus pentachloride

isopropyl ether

→

title compound

수율 106.0%

2-(5-amino-1,2,4-thiadiazol-3-yl)-2-fluoromethoxyiminoacetyl chloride . hydrochloride

수율 106.0%

용매

methylene chloride

반응 조건

후처리

1. 1
   기타to precipitate crystals
2. 2
   여과The resulting crystals were collected by filtration
3. 3
   세척washed with 20 ml of isopropyl ether
4. 4
   기타dried

실험 절차

In 50 ml of methylene chloride, 10.0 g (0.044 mol) of 2-(5-amino-1,2,4-thiadiazol-3-yl)-2-fluoromethoxyiminoacetic acid hydrate were suspended, followed by the addition of 13.3 g (0.064 mol) of phosphorus pentachloride at -20° C. After stirring for 30 minutes, 100 ml of isopropyl ether were added dropwise to the reaction mixture to precipitate crystals. The resulting crystals were collected by filtration, washed with 20 ml of isopropyl ether and then dried, whereby 9.33 g of a title compound were obtained (yield: 77%, purity: 89.7%).

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