HRID465548

反应详情

EQUATION

反应方程式

HRID 465548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 0.378 g of 2,2-dimethylpropanol in 3 ml tetrahydrofuran is added 0.003 ml of 2.5M n-butyllithium in hexane. To this solution is added 0.332 g methyl 8-(p-chlorophenylsulfonamido)-4-[3-(3-pyridyl)propyl]-octanoate and the mixture is refluxed for 20 h. The reaction is quenched by addition of 3 ml of saturated ammonium chloride solution. It is then extracted with methylene chloride (3×10 ml). The combined organic extracts are dried, filtered and evaporated to dryness to give a clear oil which is purified by preparative thin layer chromatography to obtain 2,2-dimethylpropyl 8-(p-chlorophenylsulfonamido)-4-[3-(3-pyridyl)propyl]-octanoate as a pale yellow oil.

WORKUP

后处理

  1. temperaturethe mixture is refluxed for 20 h
  2. customThe reaction is quenched by addition of 3 ml of saturated ammonium chloride solution
  3. extractionIt is then extracted with methylene chloride (3×10 ml)
  4. customThe combined organic extracts are dried
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customto give a clear oil which
  8. customis purified by preparative thin layer chromatography