HRID215988

反应详情

EQUATION

反应方程式

HRID 215988 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

Meldrum's acid (1.05 g, 7.3 mmol) was added to triethyl orthoformate (50 ml) and stirred at 30° C. for 1 hr. The reaction mixture was cooled to room temperature and 4-phenyl-thiophene-2-yl-amine (1.07 g, 6.1 mmol) was added in portions. The reaction mixture was heated to 85° C. and stirred at this temperature overnight before cooling to room temperature. The solvent was removed in vacuo to give a residue which was dissolved in DCM and treated with potassium carbonate. After stirring for 30 min the mixture was filtered and the solvent removed in vacuo to give 2,2-dimethyl-5-[(4-phenyl-thiophen-2-ylamino)-methylene]-[1,3]dioxane-4,6-dione. Yield=1.41 g (70%).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. temperatureThe reaction mixture was heated to 85° C.
  3. stirringstirred at this temperature overnight
  4. temperaturebefore cooling to room temperature
  5. customThe solvent was removed in vacuo
  6. customto give a residue which
  7. stirringAfter stirring for 30 min the mixture
  8. filtrationwas filtered
  9. customthe solvent removed in vacuo