HRID2210211

反应详情

EQUATION

反应方程式

HRID 2210211 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2.2 g (0.0139 mole) 3,4,4-trifluoro-3-butenoyl chloride is added to a mixture of 3-aminobenzoic acid (1.37 g, 0.01 mole), sodium bicarbonate (0.84 g, 0.01 mole), water (20 mL) and dichloromethane (20 mL) with stirring at 0° C. After stirring for 15 min at room temperature, the mixture is diluted with ethyl acetate (100 mL) and water (50 mL). The organic layer is washed with 2N HCl and brine, and dried. The residue obtained after evaporation of the solvent is triturated with dry ether and filtered to give 1.8 g of the title compound as a light pink solid, a 69% yield. m.p. 252°-255° C.

WORKUP

后处理

  1. stirringAfter stirring for 15 min at room temperature
  2. washThe organic layer is washed with 2N HCl and brine
  3. customdried
  4. customThe residue obtained
  5. customafter evaporation of the solvent
  6. customis triturated with dry ether
  7. filtrationfiltered