HRID1869784

反应详情

EQUATION

反应方程式

HRID 1869784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 2-amino-3-(4-nitrophenyl)propanoate 2 (9.5 g) in CH2Cl2 (40 ml) is added, at 0° C., 2,6-dichlorobenzoyl chloride (7.71 g) dissolved in CH2Cl2 (40 ml). DIPEA (2 equ.) is then added dropwise to the mixture at 0° C. The reaction is then risen at RT and pH is brought to 7-8 by addition of DIPEA. The mixture is stirred for 2 h, then evaporated and the residue is placed in AcOEt (175 ml). The organic phase is washed one time with 5% NaHCO3 (150 ml), one time with water, one time with 10% KHSO4 (150 ml) and one time with brine, dried over MgSO4 and evaporated. No further purification is needed.

WORKUP

后处理

  1. customis then risen at RT
  2. customevaporated
  3. washThe organic phase is washed one time with 5% NaHCO3 (150 ml), one time with water, one time with 10% KHSO4 (150 ml) and one time with brine
  4. dry with materialdried over MgSO4
  5. customevaporated
  6. customNo further purification