反応 #1248587

反応方程式

4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamine

8-methoxy-4H-benzo[1,3]dioxine-6-carbaldehyde

trimethylsilyl cyanide

→

title compound

(8-methoxy-4H-benzo[1,3]dioxin-6-yl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]acetonitrile

溶媒

THF

反応条件

後処理

1. 1
   ろ過The reaction mixture was filtered through celite
2. 2
   洗浄the celite was washed with 1000 ml of ethyl acetate
3. 3
   濃縮The organic layer was concentrated under reduced pressure

実験手順

To a solution of 3.5 g of Yb(OTf)3 in 250 ml of THF there were added 9.8 g of 4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamine, 10.8 g of 8-methoxy-4H-benzo[1,3]dioxine-6-carbaldehyde, 10 g of MS3A and 15 ml of trimethylsilyl cyanide under a nitrogen atmosphere, and the mixture was stirred overnight at room temperature. The reaction mixture was filtered through celite, and the celite was washed with 1000 ml of ethyl acetate. The organic layer was concentrated under reduced pressure to give the title compound (29.2 g, crude product) as a light yellow solid.

出典