HRID1799443

反应详情

EQUATION

反应方程式

HRID 1799443 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Aminoethanol (4 g, 65.48 mmol, 1 equiv) was dissolved in 200 mL of methanol, and triethylamine (9.94 g, 98.23 mmol, 1.5 equiv) was added, followed by adding ethyl trifluoroacetate (11.16 g, 78.59 mmol, 1.2 equiv). After the reaction mixture was stirred overnight at room temperature, the solvent was evaporated, and the residue was dissolved in DI water and extracted with ethyl acetate. The crude product was purified by silica gel column chromatography using ethyl acetate as eluent. The obtained product was a white solid (9.8 g, 62.42 mmol, 95% yield). 1H-NMR (600 MHz, CDCl3): δ 2.07 (s, 1H, CF3CONHCH2CH2OH); δ 3.5 (t, 2H, CF3CONHCH2CH20H); δ 3.8 (t, 2H, CF3CONHCH2CH2OH); δ 6.9 (s, 1H, CF3CONHCH2CH2OH).

WORKUP

后处理

  1. customthe solvent was evaporated
  2. dissolutionthe residue was dissolved in DI water
  3. extractionextracted with ethyl acetate
  4. customThe crude product was purified by silica gel column chromatography