反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Triethylamine (22 mmol) was added to a suspension of 4-Nitrophenylalanine methyl ester hydrochloride (2) (21 mmol) in THF (50 ml). The mixture was stirred at room temperature for one hour, the triethylamine hydrochloride was filtered off, and the filtrate concentrated to yellow oil. The oil was dissolved in dry THF (50 ml) and to this solution was added triethylamine (60 mmol) and methylbromoacetate (60 mmol), the solution was stirred at room temperature under nitrogen atmosphere for 3 hours, after which the precipitate was filtered off and the filtrate concentrated on vacuum. The residue was dissolved in ethylacetate, washed with H2O, dried (MgSO4) and concentrated on vacuum to give yellow oil. The yield was 92%.
WORKUP
后处理
- filtrationthe triethylamine hydrochloride was filtered off
- concentrationthe filtrate concentrated to yellow oil
- dissolutionThe oil was dissolved in dry THF (50 ml) and to this solution
- stirringthe solution was stirred at room temperature under nitrogen atmosphere for 3 hours
- filtrationafter which the precipitate was filtered off
- concentrationthe filtrate concentrated on vacuum
- dissolutionThe residue was dissolved in ethylacetate
- washwashed with H2O
- dry with materialdried (MgSO4)
- concentrationconcentrated on vacuum
- customto give yellow oil