HRID6320

反应详情

EQUATION

反应方程式

HRID 6320 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 3.0 g of 4-(9-decenyloxy)benzoic acid prepared in the same manner as in 9.(2) in Example 9 added was toluene, and the mixture was cooled in an ice bath. 2.0 g of thionyl chloride was added dropwise to the mixture. Subsequently, reaction was carried out for 3 hours at 80° C. After conclusion of the reaction, the product was concentrated to obtain an acid chloride compound. While, 1.7 g of 2-fluorooctyl 4-hydroxybenzoate and 0.9 g of pyridine were dissolved in toluene, and the resulting solution was cooled in an ice bath. Added dropwise thereto was a toluene solution of the above-described acid chloride compound. Reaction was then carried out for 15 hours at room temperature. After conclusion of the reaction, the product was washed with water and dried over magnesium sulfate, and the solvent was then distilled out from the dried product under reduced pressure. The residue was purified by column chromatography to obtain 2.8 g of the objective ester compound. (Yield: 85%)

WORKUP

后处理

  1. temperaturethe resulting solution was cooled in an ice bath
  2. additionAdded dropwise
  3. customReaction
  4. customAfter conclusion of the reaction
  5. washthe product was washed with water
  6. dry with materialdried over magnesium sulfate
  7. distillationthe solvent was then distilled out from the dried product under reduced pressure
  8. customThe residue was purified by column chromatography