HRID2050569

反应详情

EQUATION

反应方程式

HRID 2050569 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe excess solvent was evaporated
  2. additionthe residue treated with sodium bicarbonate solution
  3. extractionThe basic mixture was thoroughly extracted with chloroform
  4. customThe organic phase was separated
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customto leave a colorless oil which
  9. customgave a white precipitate when
  10. customThe white precipitate was recrystallised