反応 #74854

反応方程式

alpha-(N-chloroacetyl-2-methyl-6-ethylphenylamino)acetaldehyde

hydroxylamine hydrochloride

sodium bicarbonate

→

yellow oil

収率 51.2%

alpha-(N-chloroacetyl-2-methyl-6-ethylphenylamino)acetaldehyde oxime

収率 51.2%

溶媒

ethanol

反応条件

後処理

1. 1
   ろ過The reaction mixture was filtered
2. 2
   その他evaporated under reduced pressure
3. 3
   workup.ADDITIONdiluted with ethyl ether
4. 4
   ろ過filtered again
5. 5
   その他evaporated under reduced pressure

実験手順

A solution of 5 g (0.2 mol) alpha-(N-chloroacetyl-2-methyl-6-ethylphenylamino)acetaldehyde, 3.3 g (0.04 mol) hydroxylamine hydrochloride and 3.4 g (0.04 mol) sodium bicarbonate in 50 ml ethanol was heated at 40° C. for 40 minutes. The reaction mixture was filtered, evaporated under reduced pressure, diluted with ethyl ether, filtered again and evaporated under reduced pressure to give 5.5 g of a yellow oil which crystallized to a solid on standing. The crude solid was recrystallized from ethyl ether/hexane to give 3.2 g of the product as a white solid, m.p. 113°-115° C. The product is tabulated in Table I as Compound No. 11.

出典