反応 #1248570

反応方程式

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

Yb(OTf)3

trimethylsilyl cyanide

4-methoxy-3-triisopropylsilanyloxybenzaldehyde

→

solid

(4-methoxy-3-triisopropylsilanyloxyphenyl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]acetonitrile

溶媒

dichloromethane

反応条件

後処理

1. 1
   ろ過The reaction mixture was filtered
2. 2
   濃縮the filtrate was concentrated under reduced pressure
3. 3
   その他The residue was purified by silica gel column chromatography (ethyl acetate-heptane)

実験手順

After adding 3.19 g of 4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamine, 10 g of MS3A, 1.56 g of Yb(OTf)3 and 4.84 ml of trimethylsilyl cyanide to a solution of 5.6 g of 4-methoxy-3-triisopropylsilanyloxybenzaldehyde [CAS No. 179260-96-6] in 98 ml of dichloromethane under a nitrogen atmosphere, the mixture was stirred at room temperature for 12 hours. The reaction mixture was filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate-heptane) to give a white solid (5.59 g).

出典