반응 #62953

반응 방정식

3,5-difluorobenzylamine

methyl chloroacetate

triethylamine

→

N-(3,5-difluorobenzyl)glycine methyl ester

수율 41.0%

용매

dimethylformamide

ether

반응 조건

후처리

1. 1
   여과the triethylamine hydrochloride filtered
2. 2
   농축The filtrate was concentrated under vacuum
3. 3
   기타the resultant oil triturated with ethyl acetate
4. 4
   기타the solution decanted from a small amount of residual oil
5. 5
   기타The solvent was removed
6. 6
   기타the product was purified by flash chromatography (silica)
7. 7
   세척by eluting with hexane-ethyl acetate (70:30)

실험 절차

A solution of 3,5-difluorobenzylamine prepared as above (12.3 g, 0.0863 mole), methyl chloroacetate (7.6 ml, 0.0863 mole) and triethylamine (12.0 ml, 0.0863 mole) in dry dimethylformamide (85 ml) was heated at 60° C. for 3 hours. The mixture was diluted with an equal volume of ether and the triethylamine hydrochloride filtered. The filtrate was concentrated under vacuum, the resultant oil triturated with ethyl acetate, and the solution decanted from a small amount of residual oil. The solvent was removed and the product was purified by flash chromatography (silica) by eluting with hexane-ethyl acetate (70:30) to give N-(3,5-difluorobenzyl)glycine methyl ester as an oil (7.61 g, 41%).

출처