تفاعل #62953

معادلة التفاعل

3,5-difluorobenzylamine

methyl chloroacetate

triethylamine

→

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

المردود 41.0%

المذيبات

dimethylformamide

ether

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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%).

المصدر