HRID574133

反应详情

EQUATION

反应方程式

HRID 574133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of phenacylbromide (5.21 g, 26.1 mmol) in toluene (16 mL) was added over 15 minutes to a boiling, stirred solution of 1-(3,4-dihydro-2-naphthyl)pyrrolidine (5.21 g, 26.2 mmol) in toluene (17 mL). The reaction was refluxed 3 hours, diluted with water (15 mL) and refluxed for 4 hours then cooled. The layers were separated and the aqueous phase was extracted with toluene and dried over MgSO4 and concentrated. The material was purified by MPLC using a gradient from 0 to 20% ethyl acetate/hexanes to afford 4.85 g (70% yield) title product as a yellow oil.

WORKUP

后处理

  1. temperatureThe reaction was refluxed 3 hours
  2. temperaturerefluxed for 4 hours
  3. temperaturethen cooled
  4. customThe layers were separated
  5. extractionthe aqueous phase was extracted with toluene
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated
  8. customThe material was purified by MPLC