HRID2104101
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture was cooled to room temperature
- temperatureThe reaction mixture was heated to 85° C.
- stirringstirred at this temperature overnight
- temperaturebefore cooling to room temperature
- customThe solvent was removed in vacuo
- customto give a residue which
- stirringAfter stirring for 30 min the mixture
- filtrationwas filtered
- customthe solvent removed in vacuo