HRID1357294
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed under nitrogen for 19 h (overnight)
- customThe solvent was removed under reduced pressure
- customto give a red solid
- temperatureheated until most of the solid
- dissolutiondissolved
- filtrationThe mixture was filtered
- extractionextracted three times with ethyl acetate
- dry with materialdried (MgSO4)
- customthe solvent removed under reduced pressure