HRID1890810

反应详情

EQUATION

反应方程式

HRID 1890810 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(2-Fluorophenyl)hydrazine hydrochloride (1.00 g, 6.15 mmol) was suspended in ethanol (10 mL), treated with ethyl 3-amino-3-ethoxyacrylate hydrochloride (1.20 g, 6.15 mmol, 1.00 equiv), and placed into a preheated oil bath at 70° C. for 5 hours. The mixture was cooled to ambient temperature, poured into saturated aqueous sodium bicarbonate (100 mL), and extracted with ethyl acetate (3×75 mL). The combined organic extracts were dried with sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by silica gel chromatography (100:0 to 0:100 hexanes:ethyl acetate), providing the titled compound.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×75 mL)
  2. dry with materialThe combined organic extracts were dried with sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by silica gel chromatography (100:0 to 0:100 hexanes:ethyl acetate)