HRID462739

反应详情

EQUATION

反应方程式

HRID 462739 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 2-(2-fluorobenzoyl)-1-phthalimidopyrrole (12.5 g, 27 mmole) in 40 ml DMF was added 40 ml methylamine (40% solution in water). After stirring one hour at ambient temperature, the reaction mixture was diluted with water and extracted with ether. The organic extract was washed with water and with saturated NaCl solution, dried over anhydrous MgSO4, filtered and evaporated to 9 g oil, half of which was purified by Kugelrohr distallation (120°-130° at 0.2 mm Hg) to give 3.5 g (93%) solid, m.p. 44°-47°.

WORKUP

后处理

  1. extractionextracted with ether
  2. extractionThe organic extract
  3. washwas washed with water and with saturated NaCl solution
  4. dry with materialdried over anhydrous MgSO4
  5. filtrationfiltered
  6. customevaporated to 9 g oil, half of which
  7. customwas purified by Kugelrohr distallation (120°-130° at 0.2 mm Hg)