HRID880426

反应详情

EQUATION

反应方程式

HRID 880426 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Piperidine (2.45 g, 0.056 mol) was added drop wise over a period of 10 min to a stirred solution of thiophene-2-carbaldehyde (4.00 g, 0.036 mol) and malonic acid (1.00 g, 0.18 mol) in pyridine (40 mL) at 0° C. and the resulting reaction mixture was refluxed for 2 h. The reaction mixture was poured into 2N HCl (100 mL) and the precipitated solid filtered. The aqueous layer was extracted with ethyl acetate and the organic layer was washed with brine solution, dried over anhydrous sodium sulphate and concentrated under reduced pressure to afford 3-(2-thienyl)prop-2-enoic acid (5.00 g, 92%) as a solid.

WORKUP

后处理

  1. customthe resulting reaction mixture
  2. temperaturewas refluxed for 2 h
  3. filtrationthe precipitated solid filtered
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. washthe organic layer was washed with brine solution
  6. dry with materialdried over anhydrous sodium sulphate
  7. concentrationconcentrated under reduced pressure