HRID384007

反应详情

EQUATION

反应方程式

HRID 384007 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a reaction vessel, 2-[4-(2-hydroxy-ethyl)-phenyl]-2-methyl-propionic acid ethylester (25 g) prepared in the Example 4 and dichloromethane (200 mL) were introduced, and then 2-amino-2-methyl-1-propanol (10.6 mL) was introduced, and potassium t-butoxide (11.9 g) was slowly introduced. After the reaction was completed, distilled water (100 mL) was introduced to separate a layer, and the organic layer was condensed under reduced pressure. To the condensed organic layer, acetonitrile (150 mL) was added, and thionyl chloride (16 mL) was added dropwise, and then, the mixture was stirred to complete the reaction. After the reaction was completed, the mixture was cooled and sodium hydroxide solution was slowly added thereto to control pH from 5 to 7. Then, an organic solvent was removed by condensation, distilled water (150 mL) and dichloromethane (150 mL) were added thereto to separate layers. The separate organic layer was condensed under reduced pressure to obtain 2-{1-[4-(2-chloro-ethyl)-phenyl]-1-methyl-ethyl}-4,4-dimethyl-4,5-dihydro-oxazole (22.5 g, yield 80%).

WORKUP

后处理

  1. additionwere introduced
  2. distillationdistilled water (100 mL)
  3. additionwas introduced
  4. customto separate a layer
  5. customcondensed under reduced pressure
  6. customthe reaction
  7. temperaturethe mixture was cooled
  8. customThen, an organic solvent was removed by condensation
  9. distillationdistilled water (150 mL) and dichloromethane (150 mL)
  10. additionwere added
  11. customto separate layers
  12. customcondensed under reduced pressure