반응 #4225

반응 방정식

2-amino-2,3-dimethyl-butyric acid amide

triethylamine

monoethyl 2,3-dimethylfumarate chloride

→

monoethyl-2,3-dimethylfumarate N-(1-aminocarbonyl-1-methylisobutyl)-amide

수율 42.3%

용매

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture was stirred for 2 hours at room temperature
2. 2
   추출the resulting solution was extracted with water, with 2N hydrochloric acid and again with water
3. 3
   기타dried
4. 4
   기타evaporated
5. 5
   기타The residue was triturated with diethyl ether
6. 6
   여과suction-filtered
7. 7
   기타recrystallized from a little ethanol

실험 절차

A solution of 13 g of monoethyl 2,3-dimethylfumarate chloride in 20 ml of methylene chloride was added dropwise, while stirring and cooling with ice, to a solution of 12 g of 2-amino-2,3-dimethyl-butyric acid amide and 12 ml of triethylamine in 80 ml of methylene chloride. The mixture was stirred for 2 hours at room temperature, the resulting solution was extracted with water, with 2N hydrochloric acid and again with water, then dried and evaporated. The residue was triturated with diethyl ether, suction-filtered and recrystallized from a little ethanol. 8.0 g (41% of theory) of monoethyl-2,3-dimethylfumarate-N-(1-aminocarbonyl-1-methylisobutyl)-amide were obtained, m.p. 122°-125° C.

출처