HRID63924

反应详情

EQUATION

反应方程式

HRID 63924 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 3-(4-chlorobenzyl)-4-(3-chlorophenyl)-2-cyano-4-oxobutanoate (1.945 g, 5 mmol) in TFA (20 mL) was stirred at 100° C. for 3 h. The reaction was cooled to RT and concentrated to a residue which was diluted with EA (40 mL) and water (8 mL). The organic layer was dried over Na2SO4 and concentrated to a residue which was purified by chromatography eluted with PE/EA (5:1) to give ethyl 2-amino-4-(4-chlorobenzyl)-5-(3-chlorophenyl)furan-3-carboxylate (1.4 g, 72% yield) as a white solid. LCMS: MH+ 390 and TR=2.503 min.

WORKUP

后处理

  1. concentrationconcentrated to a residue which
  2. additionwas diluted with EA (40 mL) and water (8 mL)
  3. dry with materialThe organic layer was dried over Na2SO4
  4. concentrationconcentrated to a residue which
  5. customwas purified by chromatography
  6. washeluted with PE/EA (5:1)