반응 #452253

반응 방정식

water

methyl 2-formylbenzoate

2-amino-2,3-dimethylbutyramide

p-toluenesulfonic acid

→

methyl o-[N-(1-carbamoyl-1,2-dimethylpropyl)formimidoyl]benzoate

용매

toluene

반응 조건

후처리

1. 1
   온도is heated
2. 2
   여과The mixture is filtered
3. 3
   농축concentrated in vacuo
4. 4
   기타The residue crystallizes on standing
5. 5
   기타is recrystallized from etherhexane

실험 절차

A mixture containing 5.0 g methyl 2-formylbenzoate [C. Brown and M. V. Sargent, J. Chem. Soc. (C), 1818 (1969)] and 4.0 g 2-amino-2,3-dimethylbutyramide and 50 mg p-toluenesulfonic acid in 100 mL toluene is heated under reflux under a Dean-Stark water separator for three hours. The mixture is filtered and concentrated in vacuo. The residue crystallizes on standing and is recrystallized from etherhexane to give analytically pure methyl o-[N-(1-carbamoyl-1,2-dimethylpropyl)formimidoyl]benzoate, mp 79°-80.5° C.

출처