HRID1355427

反应详情

EQUATION

反应方程式

HRID 1355427 的结构方程式

PROCEDURE

实验过程

2-Methyl-3-phenylthiopropanal (9.07 g, 0.05 mole), 3-buten-2-ol (18.04 g, 0.25 mole), and p-toluenesulfonic acid (0.24 g, 0.0013 mole) are added to 90 ml of xylenes. The reaction mixture is heated to reflux using a Dean-Stark trap to collect water. After 3 hours, the mixture is cooled to room temperature and quenched with 30 ml of saturated NaHCO3 solution. The two phases are separated and the aqueous phase is extracted with 30 ml of ethyl acetate. The combined organic extracts is washed with 20 ml of brine and dried with Na2SO4. After removing solvents, the crude product is purified by chromatography. The product is obtained in 74.3% as a colorless oil.

WORKUP

后处理

  1. temperatureThe reaction mixture is heated
  2. temperatureto reflux
  3. customto collect water
  4. customquenched with 30 ml of saturated NaHCO3 solution
  5. customThe two phases are separated
  6. extractionthe aqueous phase is extracted with 30 ml of ethyl acetate
  7. washThe combined organic extracts is washed with 20 ml of brine
  8. dry with materialdried with Na2SO4
  9. customAfter removing solvents
  10. customthe crude product is purified by chromatography
  11. customThe product is obtained in 74.3% as a colorless oil