HRID2050569
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
Isobutyryl bromide (12 g) was added to a stirred solution of 4-[2-(6-(2-Phenylethylamino)hexylamino) ethyl]-1,2-benzenediol dihydrobromide (4 g) in trifluoracetic acid (100 ml). The solution was then stirred at room temperature for 24 hours. The excess solvent was evaporated and the residue treated with sodium bicarbonate solution. The basic mixture was thoroughly extracted with chloroform. The organic phase was separated, dried over magnesium sulfate, filtered and evaporated to leave a colorless oil which gave a white precipitate when treated with ethereal HCl. The white precipitate was recrystallised to give the title compound from ethanol as colorless prisms (2.8 g), m.p. 232°-234°.
WORKUP
后处理
- customThe excess solvent was evaporated
- additionthe residue treated with sodium bicarbonate solution
- extractionThe basic mixture was thoroughly extracted with chloroform
- customThe organic phase was separated
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customevaporated
- customto leave a colorless oil which
- customgave a white precipitate when
- customThe white precipitate was recrystallised