HRID2260460

反应详情

EQUATION

反应方程式

HRID 2260460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a 500 mL round bottomed flask equipped with a magnetic stirrer, condenser and nitrogen atmosphere are charged 2.0 g (4.2 mmol) of 2,4-bis-(2,4-dihydroxyphenyl)-6-[4-(phenylthio)phenyl]-s-triazine, 0.58 g (4.2 mmol) of potassium carbonate and 30 mL of N,N-dimethylformamide. The mixture is heated to 90° C., and the s-triazine compound dissolves readily. Bromobutane (4.5 mL, 42.0 mmol) is added all at once. The reaction mixture is heated at 90° C. for 2.5 hours and then stirred at room temperature overnight yielding a yellow precipitate. Chilled water is added and the yellow precipitate is isolated by vacuum filtration to give 2.74 g of crude product. The crude product is purified by flash chromatography with 1:1 heptane:ethyl acetate to afford 0.26 g (10%) yield of the title compound as a yellow solid; mp>250°.

WORKUP

后处理

  1. customTo a 500 mL round bottomed flask equipped with a magnetic stirrer, condenser
  2. temperatureThe reaction mixture is heated at 90° C. for 2.5 hours
  3. customyielding a yellow precipitate
  4. customthe yellow precipitate is isolated by vacuum filtration
  5. customto give 2.74 g of crude product
  6. customThe crude product is purified by flash chromatography with 1:1 heptane