HRID2073429

反应详情

EQUATION

反应方程式

HRID 2073429 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.08 mg of 3-trifluoromethyl-1-nonanol was dissolved in 453 mg of pyridine, and the solution was cooled with ice, followed by addition of 276 mg of p-toluenesulfonic chloride, stirring for 2 hours under cooling with ice and stirring overnight at room temperature. After the reaction, the product was acidified with 2N-hydrochloric acid and extracted with diethyl ether. The resultant diethyl ether solution was washed with water and dried with magnesium sulfate, and the solvent was distilled off. The crude product was purified by thin layer chromatography with benzene as the developer to obtain 345 mg (yield: 65%) of 3-trifluoromethylnonyl p-toluenesulfonate, which showed: [α]D28 +1.63 (c 5.04, CHCl3).

WORKUP

后处理

  1. temperaturethe solution was cooled with ice
  2. temperatureunder cooling with ice
  3. stirringstirring overnight at room temperature
  4. customAfter the reaction
  5. extractionextracted with diethyl ether
  6. washThe resultant diethyl ether solution was washed with water
  7. dry with materialdried with magnesium sulfate
  8. distillationthe solvent was distilled off
  9. customThe crude product was purified by thin layer chromatography with benzene as the developer