HRID1349938

反应详情

EQUATION

反应方程式

HRID 1349938 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

tert-Butyl 4-[2-(2-methylquinolin-5-yloxy)ethyl]piperazine-1-carboxylate (1.04 g, 2.8 mmol) was dissolved in ethanol (60 mL) and treated with 1M hydrochloric acid in diethyl ether (16 mL, 16 mmol) and stirred at 40° C. for 17 h. The reaction mixture was filtered and the white solid was collected and dried in vacuo. The hydrochloride salt precipitate was dissolved in water (25 mL) and potassium carbonate was added until the pH reached 10. The aqueous layer was washed with 5% methanol in dichloromethane (4×100 mL) then 10% methanol in dichloromethane (4×100 mL). The organic layers were combined, dried (Na2SO4) and concentrated in vacuo, affording the title compound as a brown oil (0.69 g, 91%).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. customthe white solid was collected
  3. customdried in vacuo
  4. dissolutionThe hydrochloride salt precipitate was dissolved in water (25 mL)
  5. additionpotassium carbonate was added until the pH
  6. washThe aqueous layer was washed with 5% methanol in dichloromethane (4×100 mL)
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated in vacuo