반응 #2501231

반응 방정식

methanol

N-neopentyl-N-2-propinyloxycarbonyloxamic acid chloride

triethylamine

→

methyl N-neopentyl-N-2-propinyloxycarbonyl-oxamate

수율 98.0%

용매

toluene

반응 조건

후처리

1. 1
   workup.ADDITIONare then added dropwise
2. 2
   온도while cooling with ice
3. 3
   여과After the precipitate has been filtered off
4. 4
   세척the filtrate is washed with water
5. 5
   건조dried over sodium sulphate

실험 절차

0.64 g (0.02 mole) of methanol are added to 5.35 g (0.02 mole) of 97% pure N-neopentyl-N-2-propinyloxycarbonyloxamic acid chloride in 50 ml of toluene, and 2.02 g (0.02 mole) of triethylamine are then added dropwise, while cooling with ice. After the precipitate has been filtered off, the filtrate is washed with water, dried over sodium sulphate and freed from the solvent under a high vacuum. 5 g (98% of theory) of methyl N-neopentyl-N-2-propinyloxycarbonyl-oxamate of refractive index nD20 =1.4634 are obtained.

출처