HRID719663

反应详情

EQUATION

反应方程式

HRID 719663 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationthe triethylamine hydrochloride was filtered off
  2. concentrationthe filtrate concentrated to yellow oil
  3. dissolutionThe oil was dissolved in dry THF (50 ml) and to this solution
  4. stirringthe solution was stirred at room temperature under nitrogen atmosphere for 3 hours
  5. filtrationafter which the precipitate was filtered off
  6. concentrationthe filtrate concentrated on vacuum
  7. dissolutionThe residue was dissolved in ethylacetate
  8. washwashed with H2O
  9. dry with materialdried (MgSO4)
  10. concentrationconcentrated on vacuum
  11. customto give yellow oil