반응 #470381

반응 방정식

L-lysine methyl ester dihydrochloride

triethylamine

benzyloxy acetyl chloride

→

2

수율 31.8%

2,6-Bis-(2-benzyloxy-acetylamino)-hexanoic acid methyl ester

수율 31.8%

용매

ethyl acetate

반응 조건

후처리

1. 1
   여과The solids were filtered off
2. 2
   세척The organic phase was washed with 5% sodium bicarbonate (2×100 mL), water (2×100 mL)
3. 3
   건조dried over sodium sulphate
4. 4
   workup.DISTILLATIONdistilled
5. 5
   기타The crude 2 was purified by column chromatography on silica gel

실험 절차

To a mixture of L-lysine methyl ester dihydrochloride (50 grams, 214.4 mmol), triethylamine (131 grams, 1.294 moles) in ethyl acetate (750 mL) at room temperature was added benzyloxy acetyl chloride (120 grams, 650.4 mmol) drop wise. The mixture was further stirred at room temperature for 2 hours. The solids were filtered off. The organic phase was washed with 5% sodium bicarbonate (2×100 mL), water (2×100 mL), dried over sodium sulphate and distilled. The crude 2 was purified by column chromatography on silica gel using Benzene: Ethyl acetate (9:1) to get pure 2 (30 grams, 31.8%) as a white powder.

출처