HRID38274

反应详情

EQUATION

反应方程式

HRID 38274 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of DCC (5.07 g) in DCM (140 mL) at 0° C. was added N—BOC-L-□-aminobutyric acid (5 g) followed by ethyl JV-benzylglycinate (4.6 mL) dropwise. The resulting solution was stirred at 0° C. for 2 h and RT 1 h, filtered and the concentrated to give an oil. This was dissolved in DCM (100 mL) and TFA (100 ml) and stirred for 1 h. The solution was concentrated under reduced pressure. The residue was stirred in saturated aq NaHCO3 (125 ml) and EtOAc (125 ml) for 6 h. The organics were separated, dried (Na2SO4), and concentrated to give the sub title compound as a white solid. (5.68 g).

WORKUP

后处理

  1. filtrationfiltered
  2. concentrationthe concentrated
  3. customto give an oil
  4. concentrationThe solution was concentrated under reduced pressure
  5. stirringThe residue was stirred in saturated aq NaHCO3 (125 ml)
  6. waitEtOAc (125 ml) for 6 h
  7. customThe organics were separated
  8. dry with materialdried (Na2SO4)
  9. concentrationconcentrated