反応 #4225

反応方程式

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

triethylamine

monoethyl 2,3-dimethylfumarate chloride

→

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

収率 42.3%

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   workup.STIRRINGThe mixture was stirred for 2 hours at room temperature
2. 2
   抽出the resulting solution was extracted with water, with 2N hydrochloric acid and again with water
3. 3
   その他dried
4. 4
   その他evaporated
5. 5
   その他The residue was triturated with diethyl ether
6. 6
   ろ過suction-filtered
7. 7
   その他recrystallized from a little ethanol

実験手順

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.

出典