HRID1093035

反应详情

EQUATION

反应方程式

HRID 1093035 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 ethyl 2-((2-fluoroethyl)(methyl)amino)-2-oxoacetate (1.2 g, 7.36 mmol) in methanol/water (30 mL, 1:1) was added LiOH (0.352 g, 14.71 mmol). The solution was stirred for 2 h. The methanol was removed by concentration and concentrated HCl (2 mL) was added. The solvent was removed and the residue dissolved in CH2Cl2 and filtered. The filtrate was concentrated to give the title compound as an off-white crystalline powder (0.615 g, 56% yield). 1H NMR (400 MHz, CDCl3) δ: 4.47-4.89 (2 H, m) 3.67-4.39 (2 H, m) 3.07-3.60 (3 H, m).

WORKUP

后处理

  1. customThe methanol was removed by concentration and concentrated HCl (2 mL)
  2. additionwas added
  3. customThe solvent was removed
  4. dissolutionthe residue dissolved in CH2Cl2
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated