反应 #470381
ord-eafcc244dfa248c5ba85114b659eccac
反应方程式
L-lysine methyl ester dihydrochloride
triethylamine
benzyloxy acetyl chloride
→
2
收率 31.8%
2,6-Bis-(2-benzyloxy-acetylamino)-hexanoic acid methyl ester
收率 31.8%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1过滤The solids were filtered off
- 2洗涤The organic phase was washed with 5% sodium bicarbonate (2×100 mL), water (2×100 mL)
- 3干燥dried over sodium sulphate
- 4workup.DISTILLATIONdistilled
- 5其他The crude 2 was purified by column chromatography on silica gel
实验过程
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.