反応 #50757

反応方程式

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

phosphorus pentachloride

isopropyl ether

→

title compound

収率 106.0%

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

収率 106.0%

溶媒

methylene chloride

反応条件

後処理

1. 1
   その他to precipitate crystals
2. 2
   ろ過The resulting crystals were collected by filtration
3. 3
   洗浄washed with 20 ml of isopropyl ether
4. 4
   その他dried

実験手順

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%).

出典