HRID383984

反应详情

EQUATION

反应方程式

HRID 383984 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 12.5 g (51.4 mmol) of N-(4-fluorophenethyl)benzamide and polyphosphoric acid (150 ml) was heated at 150° C. for 5 days. Then the hot solution was poured into water and the reaction was quenched by the addition of NaHCO3. It was extracted with DCM (3×300 ml). The combined organic phases were washed with brine (300 ml), dried over Na2SO4, filtered and concentrated to small volume under vacuum. 3.2 g of the crude product 7-fluoro-1-phenyl-3,4-dihydroisoquinoline were obtained as the residue, which was reacted further with no additional purification.

WORKUP

后处理

  1. customthe reaction was quenched by the addition of NaHCO3
  2. extractionIt was extracted with DCM (3×300 ml)
  3. washThe combined organic phases were washed with brine (300 ml)
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated to small volume under vacuum