HRID1699736

反应详情

EQUATION

反应方程式

HRID 1699736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

3.08 g of the 5-hydroxymethyl-3-iodobenzoic acid methyl ester obtained in the production example 2 was dissolved in 50 ml of dry DMF under the flow of nitrogen and then mixed with 2.32 g of the compound in the production example 3, 2.18 g of potassium carbonate and 456 mg of tetrakis(triphenylphosphine) palladium (0). The obtained mixture solution was heated and stirred at 90° C. overnight, mixed with water to stop the reaction, and then extracted with ethyl acetate. The obtained ethyl acetate layer was dried over MgSO4, and the solvent was distilled away. The residue was purified by silica gel column chromatography to obtain 2.05 g (73%) of the title compound. Colorless crystals.

WORKUP

后处理

  1. temperatureThe obtained mixture solution was heated
  2. customthe reaction
  3. extractionextracted with ethyl acetate
  4. dry with materialThe obtained ethyl acetate layer was dried over MgSO4
  5. distillationthe solvent was distilled away
  6. customThe residue was purified by silica gel column chromatography