HRID369361

反应详情

EQUATION

反应方程式

HRID 369361 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl (S)-3-[2-(tert-butoxycarbonylamino)-1,2,3,4-tetrahydronaphthalen-7-yl]acrylate (516 mg) was dissolved in ethanol (10 ml), and 3 M hydrogen chloride ethanol solution (2 ml) was added to the solution at room temperature with stirring. After reaction for 13 hours, the reaction mixture was concentrated in vacuo. A saturated aqueous sodium bicarbonate solution (20 ml) and dichloromethane (5 ml) were added to the residue, and the resulting mixture was stirred for an hour at room temperature. Water was added to the reaction mixture, and the resulting mixture was extracted with dichloromethane. The extract was washed with water and dried over anhydrous magnesium sulfate. Removal of the solvent in vacuo gave ethyl (S)-3-(2-amino-1,2,3,4-tetrahydronaphthalen-7-yl)acrylate (366 mg) as an oil.

WORKUP

后处理

  1. customAfter reaction for 13 hours
  2. concentrationthe reaction mixture was concentrated in vacuo
  3. additionA saturated aqueous sodium bicarbonate solution (20 ml) and dichloromethane (5 ml) were added to the residue
  4. stirringthe resulting mixture was stirred for an hour at room temperature
  5. additionWater was added to the reaction mixture
  6. extractionthe resulting mixture was extracted with dichloromethane
  7. washThe extract was washed with water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customRemoval of the solvent in vacuo