HRID1357294

反应详情

EQUATION

反应方程式

HRID 1357294 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of benzyl-(6-methoxy-naphthalen-2-ylmethyl)-amine (1.3 g, 4.7 mmol), prepared in the previous step, 65 mL of 48% HBr and 50 mL of glacial acetic acid was refluxed under nitrogen for 19 h (overnight). The solvent was removed under reduced pressure to give a red solid. The solid was suspended in 250 mL of water and heated until most of the solid dissolved. The mixture was filtered, the filtrate made basic with sodium bicarbonate and extracted three times with ethyl acetate. The organic extracts were combined, dried (MgSO4) and the solvent removed under reduced pressure to give 6-(benzylamino-methyl)-naphthalen-2-ol (0.76 g, 62%) as a green solid, mp 120-122° C.

WORKUP

后处理

  1. temperaturewas refluxed under nitrogen for 19 h (overnight)
  2. customThe solvent was removed under reduced pressure
  3. customto give a red solid
  4. temperatureheated until most of the solid
  5. dissolutiondissolved
  6. filtrationThe mixture was filtered
  7. extractionextracted three times with ethyl acetate
  8. dry with materialdried (MgSO4)
  9. customthe solvent removed under reduced pressure