HRID1469140

反应详情

EQUATION

反应方程式

HRID 1469140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Ethyl 5-hydroxypentanoate (1.12 g, 7.66 mmol) was dissolved in 25 mL of methylene chloride, triphosgene (772 mg, 0.34 equivalent), and pyridine (0.743 mL, 1.2 equivalent) were sequentially added while stirred at 0° C., and the mixture was stirred at room temperature for 1 hour. After completion of the reaction, water was added, and extraction operation (methylene chloride) was performed. The separated organic layer was washed using an aqueous saturated sodium chloride solution, and dried with magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain the crude product. This was purified by column chromatography (ethyl acetate:n-hexane=1:10) to obtain the title compound (972 mg) having the following physical property values.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 1 hour
  2. additionwas added
  3. extractionextraction operation (methylene chloride)
  4. washThe separated organic layer was washed
  5. dry with materialdried with magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customto obtain the crude product
  8. customThis was purified by column chromatography (ethyl acetate:n-hexane=1:10)