HRID347894

反应详情

EQUATION

反应方程式

HRID 347894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of cis-1-[2-[4-(6-methoxy-2-phenyl-1,2,3,4 tetrahydronaphthalen-1-yl)phenoxy]ethyl}pyrrolidine (12 g, 28 mmol), acetic acid (75 mL), and 48% HBr (75 mL) was heated at 100° C. for 15 h. The solution was cooled and the resulting white precipitate was collected by filtration. The hydrobromide salt (9.6 g, 69%) was dissolved in CHCl3/MeOH and was stirred with saturated NaHCO3 (aq). The layers were separated and the aqueous layer was further extracted with CHCl3/MeOH. The combined organic layers were dried (MgSO4), filtered, and concentrated to yield product as an off-white foam.

WORKUP

后处理

  1. temperatureThe solution was cooled
  2. filtrationthe resulting white precipitate was collected by filtration
  3. dissolutionThe hydrobromide salt (9.6 g, 69%) was dissolved in CHCl3/MeOH
  4. customThe layers were separated
  5. extractionthe aqueous layer was further extracted with CHCl3/MeOH
  6. dry with materialThe combined organic layers were dried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto yield product as an off-white foam